CN101891176A - Method for preparing iron phosphate by using nonionic surfactant - Google Patents
Method for preparing iron phosphate by using nonionic surfactant Download PDFInfo
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- CN101891176A CN101891176A CN 201010209297 CN201010209297A CN101891176A CN 101891176 A CN101891176 A CN 101891176A CN 201010209297 CN201010209297 CN 201010209297 CN 201010209297 A CN201010209297 A CN 201010209297A CN 101891176 A CN101891176 A CN 101891176A
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- iron phosphate
- nonionic surfactant
- tertiary iron
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Abstract
The invention belongs to the technical field of electrochemistry and in particular relates to a method for preparing iron phosphate by using a nonionic surfactant. The method comprises the following steps of: dissolving analytically pure soluble phosphate in distilled water to prepare water solution A, adding 0.05 to 5 mass percent of nonionic surfactant into the water solution A and preparing iron salt with a certain mole ratio into solution B by using deionized water; and adding the solution B into the solution A, reacting at the temperature of between 20 and 100 DEG C for 1 to 5 hours, filtering the mixed solution and drying the filtered product at the temperature of between 50 and 150 DEG C for 2 to 15 hours to obtain iron phosphate with uniform particle size and particle size of between 50 and 300 nanometers. The method of the invention has the advantages of simple synthesis process, easy industrialization and easy cleaning and no residual of nonionic surfactant in a synthesis process. Lithium ferrous phosphate prepared from the iron phosphate synthesized by the method has high electrochemical performance.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to prepare the method for tertiary iron phosphate.
Background technology
Goodenough group reported first in 1997 have a LiFePO 4 (LiFePO of olivine structural
4) can reversible embed or take off the embedding ion, be considered to the desirable positive electrode material of lithium ion battery.LiFePO
4Theoretical capacity be 170mAh/g, relatively the electrode potential of lithium is 3.5V.Under little electric current, LiFePO
4Smooth discharge voltage profile is arranged, and its voltage curve can match in excellence or beauty with voltage stabilized source.It is at present industrial that a lot of LiFePO 4s is arranged all is as the precursor synthetic with tertiary iron phosphate.
The synthetic method of tertiary iron phosphate is a lot, and the most traditional is directly with molysite and phosphoric acid or phosphate reaction, filtration washing drying.But synthetic sample particle size is inhomogeneous in this way, and reunites easily, can not well be used for the synthetic of LiFePO 4.The synthetic highdensity ball shape ferric phosphate of the ammonium citrate of use or ammonium oxalate is arranged among the Chinese patent CN 101269807A, use anionic surfactant sodium dodecylbenzene sulfonate, sodium olefin sulfonate or sodium lauryl sulphate to synthesize well behaved tertiary iron phosphate among the patent CN 101172594A.Aforesaid method can both solve present tertiary iron phosphate synthetic problem preferably, the author finds that in experiment not only particle is less with nonionogenic tenside synthetic tertiary iron phosphate, size evenly but also is used for these dispersive nonionogenic tenside flush away easily filtering the time.
Summary of the invention
The object of the present invention is to provide a kind of synthesis technique simple, realize the industrialized method for preparing tertiary iron phosphate easily.
The method for preparing tertiary iron phosphate provided by the invention adopts nonionogenic tenside, and concrete steps are as follows:
1, soluble phosphate is dissolved in distilled water, is mixed with water solution A, add the nonionogenic tenside of phosphoric acid salt quality 0.05-5%;
2, the molysite with certain mol proportion is mixed with solution B with deionized water, B solution is joined in the above-mentioned A solution again, and 20-100 ℃ of reaction 1-5h filters, and 50-150 ℃ of dry 2-15h promptly obtains even particle size, and particle diameter is the tertiary iron phosphate of 50-300nm.
In the above-mentioned reaction, PO
4 3-: Fe
3+Ratio between 1.5～1.
Above-mentioned used source of iron is a kind of in iron nitrate, ferric sulfate, iron trichloride, the ferrous sulfate, or wherein several.
Above-mentioned used nonionogenic tenside is PEG, and P123 is a kind of among the PMAA, or wherein several.
Above-mentioned used phosphoric acid salt is a kind of in phosphoric acid, primary ammonium phosphate, SODIUM PHOSPHATE, MONOBASIC, Secondary ammonium phosphate, the Sodium phosphate dibasic, or wherein several.
The present invention uses the method for the synthetic tertiary iron phosphate of nonionogenic tenside, has following advantage: the iron phosphate grains size homogeneous that synthesizes is 50-300nm.Synthesis technique is simple, is easy to industrialization.Nonionogenic tenside cleans easily in the building-up process, and is not residual.And the synthetic tertiary iron phosphate prepares LiFePO 4 and has high electrochemical performance in this way.
Embodiment
Embodiment 1:
Take by weighing a certain amount of primary ammonium phosphate and be mixed with the solution of 0.05mol/L, in above-mentioned solution, add the PEG of 0.1g, again with the FeCl of 0.05mol with the 100ml deionized water
3.6H
2O is dissolved in the distilled water of 100ml, joins in the above-mentioned ammonium dihydrogen phosphate, and reaction 2h filters, washing, and 100 ℃ of 10h oven dry obtain FePO
42H2O.
Embodiment 2:
Take by weighing a certain amount of FeCl
36H
2O is mixed with the solution of 1mo/L with the 100ml deionized water, adds the P123 of 0.5g in above-mentioned solution, and the primary ammonium phosphate with 1mol is dissolved in the distilled water of 100ml again, joins above-mentioned FeCl
36H
2In the O solution, reaction 5h filters, washing, and 80 ℃ of 10h oven dry obtain FePO
42H
2O.
Embodiment 3:
Take by weighing a certain amount of primary ammonium phosphate and be mixed with the solution of 2mol/L, in above-mentioned solution, add the PMAA of 0.1g, again with the FeCl of 2mol with the 100ml deionized water
36H
2O is dissolved in the distilled water of 100ml, joins in the above-mentioned ammonium dihydrogen phosphate, and reaction 1h filters, washing, and 50 ℃ of 15h oven dry obtain FePO
42H
2O.
Embodiment 4:
Take by weighing a certain amount of primary ammonium phosphate and be mixed with the solution of 2mol/L, in above-mentioned solution, add the PMAA of 0.5g, again with the FeSO of 2mol with the 100ml deionized water
46H
2O is dissolved in the distilled water of 100ml, joins in the above-mentioned ammonium dihydrogen phosphate, mixes, and slowly adds 1.2molH
2O
2, reaction 2h filters, washing, and 150 ℃ of 6h oven dry obtain FePO
42H
2O.
Claims (4)
1. one kind prepares the method for tertiary iron phosphate with nonionogenic tenside, it is characterized in that concrete steps are as follows:
(1) soluble phosphate is dissolved in distilled water, is mixed with water solution A, add the nonionogenic tenside of phosphoric acid salt quality 0.05-5%;
(2) molysite with certain mol proportion is mixed with solution B with deionized water, B solution is joined in the above-mentioned A solution again, and 20-100 ℃ of reaction 1-5h filters, and 50-150 ℃ of dry 2-15h promptly obtains even particle size, and particle diameter is the tertiary iron phosphate of 50-300nm;
In the above-mentioned reaction, PO
4 3-: Fe
3+Ratio between 1.5～1.
2. the method for preparing tertiary iron phosphate according to claim 1 is characterized in that used molysite is a kind of in iron nitrate, ferric sulfate, iron trichloride, the ferrous sulfate, or wherein several.
3. the method for preparing tertiary iron phosphate according to claim 1 is characterized in that used nonionogenic tenside is PEG, and P123 is a kind of among the PMAA, or wherein several.
4. the method for preparing tertiary iron phosphate according to claim 1 is characterized in that used phosphoric acid salt is a kind of in phosphoric acid, primary ammonium phosphate, SODIUM PHOSPHATE, MONOBASIC, Secondary ammonium phosphate, the Sodium phosphate dibasic, or wherein several.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010209297 CN101891176B (en) | 2010-06-24 | 2010-06-24 | Method for preparing iron phosphate by using nonionic surfactant |
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|---|---|---|---|
| CN 201010209297 CN101891176B (en) | 2010-06-24 | 2010-06-24 | Method for preparing iron phosphate by using nonionic surfactant |
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| CN101891176A true CN101891176A (en) | 2010-11-24 |
| CN101891176B CN101891176B (en) | 2013-01-02 |
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| CN 201010209297 Expired - Fee Related CN101891176B (en) | 2010-06-24 | 2010-06-24 | Method for preparing iron phosphate by using nonionic surfactant |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009968A (en) * | 2011-01-14 | 2011-04-13 | 武汉大学 | Preparation method of nano-flaky FePO4.2H2O |
| CN102009967A (en) * | 2010-12-23 | 2011-04-13 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102616763A (en) * | 2012-04-01 | 2012-08-01 | 清华大学深圳研究生院 | Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate |
| CN103208627A (en) * | 2013-02-22 | 2013-07-17 | 贵州省开阳安达磷化工有限公司 | Ferric phosphate material and manufacturing method thereof |
| CN103606676A (en) * | 2013-11-12 | 2014-02-26 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate/carbon nanocomposite and preparation method thereof |
| CN105645371A (en) * | 2016-01-08 | 2016-06-08 | 西南大学 | One-step preparation method and application of nano transition metal phosphates |
| CN108793116A (en) * | 2018-06-27 | 2018-11-13 | 内江师范学院 | The preparation method and applications of different-shape micron ferric phosphate |
| CN109052358A (en) * | 2018-10-09 | 2018-12-21 | 湖南雅城新材料有限公司 | A kind of preparation method of mesopore-macropore ferric phosphate |
| CN111153391A (en) * | 2020-01-09 | 2020-05-15 | 湖南雅城新材料有限公司 | Preparation method of low-sulfur-content battery-grade iron phosphate |
| CN112436132A (en) * | 2020-12-10 | 2021-03-02 | 桂林理工大学 | Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117216A (en) * | 2007-07-23 | 2008-02-06 | 河北工业大学 | Hydrothermal synthesis method for lithium ion-cell anode material of ferric phosphate lithium |
| CN101630739A (en) * | 2008-12-30 | 2010-01-20 | 横店集团东磁股份有限公司 | Preparation method of modification doping lithium ferric phosphate |
-
2010
- 2010-06-24 CN CN 201010209297 patent/CN101891176B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101117216A (en) * | 2007-07-23 | 2008-02-06 | 河北工业大学 | Hydrothermal synthesis method for lithium ion-cell anode material of ferric phosphate lithium |
| CN101630739A (en) * | 2008-12-30 | 2010-01-20 | 横店集团东磁股份有限公司 | Preparation method of modification doping lithium ferric phosphate |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102009967A (en) * | 2010-12-23 | 2011-04-13 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102009967B (en) * | 2010-12-23 | 2012-06-20 | 武汉大学 | Method for preparing iron phosphate with micro/nano structure |
| CN102009968B (en) * | 2011-01-14 | 2012-08-08 | 武汉大学 | Preparation method of nano-flaky FePO4.2H2O |
| CN102009968A (en) * | 2011-01-14 | 2011-04-13 | 武汉大学 | Preparation method of nano-flaky FePO4.2H2O |
| CN102616763A (en) * | 2012-04-01 | 2012-08-01 | 清华大学深圳研究生院 | Preparation method of iron phosphate for preparing lithium iron phosphate and iron phosphate |
| CN103208627B (en) * | 2013-02-22 | 2015-11-25 | 贵州安达科技能源股份有限公司 | A kind of ferric phosphate material and preparation method thereof |
| CN103208627A (en) * | 2013-02-22 | 2013-07-17 | 贵州省开阳安达磷化工有限公司 | Ferric phosphate material and manufacturing method thereof |
| CN103606676A (en) * | 2013-11-12 | 2014-02-26 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate/carbon nanocomposite and preparation method thereof |
| CN103606676B (en) * | 2013-11-12 | 2016-06-29 | 深圳市贝特瑞纳米科技有限公司 | A kind of lithium iron phosphate/carbon nanocomposite and preparation method thereof |
| CN105645371A (en) * | 2016-01-08 | 2016-06-08 | 西南大学 | One-step preparation method and application of nano transition metal phosphates |
| CN108793116A (en) * | 2018-06-27 | 2018-11-13 | 内江师范学院 | The preparation method and applications of different-shape micron ferric phosphate |
| CN109052358A (en) * | 2018-10-09 | 2018-12-21 | 湖南雅城新材料有限公司 | A kind of preparation method of mesopore-macropore ferric phosphate |
| CN111153391A (en) * | 2020-01-09 | 2020-05-15 | 湖南雅城新材料有限公司 | Preparation method of low-sulfur-content battery-grade iron phosphate |
| CN111153391B (en) * | 2020-01-09 | 2021-12-31 | 湖南雅城新材料有限公司 | Preparation method of low-sulfur-content battery-grade iron phosphate |
| CN112436132A (en) * | 2020-12-10 | 2021-03-02 | 桂林理工大学 | Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus |
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| CN101891176B (en) | 2013-01-02 |
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Application publication date: 20101124 Assignee: Gejiu Shengbihe Industrial Co., Ltd. Assignor: Fudan University Contract record no.: 2014530000049 Denomination of invention: Method for preparing iron phosphate by using nonionic surfactant Granted publication date: 20130102 License type: Exclusive License Record date: 20140520 |
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