CN106784813A - A kind of preparation method of iron manganese phosphate lithium material - Google Patents
A kind of preparation method of iron manganese phosphate lithium material Download PDFInfo
- Publication number
- CN106784813A CN106784813A CN201611062080.9A CN201611062080A CN106784813A CN 106784813 A CN106784813 A CN 106784813A CN 201611062080 A CN201611062080 A CN 201611062080A CN 106784813 A CN106784813 A CN 106784813A
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- Prior art keywords
- lithium
- iron manganese
- manganese phosphate
- preparation
- phosphate
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
-
- 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
Abstract
A kind of preparation method of iron manganese phosphate lithium material, preparation process is：(1) analytically pure phosphoric acid Asia manganese, ferrous phosphate, lithium dihydrogen phosphate, lithium carbonate in molar ratio (0.8~0.9): (0.1~0.2): 1: 1 ratio is added in hydrothermal reaction kettle, add deionized water dissolving；(2) reactor is heated into 180 DEG C to be kept for 12 hours, is then cooled to room temperature, take out whole materials, 105 DEG C of forced air dryings turn into bulk；(3) 5% carbonaceous organic material and appropriate absolute ethyl alcohol are added in block, mixed sand is milled to 100~300nm, is taken out, be then spray-dried, as 2~10 μm or so particles.(4) particle is sintered under the atmosphere such as nitrogen, 700 DEG C~800 DEG C is warmed up to the speed of 5 DEG C/min, kept for 5 hours, be naturally cooling to room temperature, taken out, obtain iron manganese phosphate for lithium.
Description
Technical field
The invention belongs to new chemical energy storage field, more particularly to a kind of preparation method of iron manganese phosphate lithium material.
Background technology
LiFePO4 is a kind of widely used power battery anode material because its security it is good and have extended cycle life and
The favor of electric automobile market is obtained, but its operating voltage is low, Fe3+/Fe2+Relative to Li+The current potential of/Li is only 3.4V, is made
The specific energy for obtaining LiFePO 4 material is low, and its development is limited to a certain extent.
Lithium manganese phosphate has the similar structure of LiFePO 4 material, but its operating voltage is higher, Fe3+/Fe2+Relative to
Li+The current potential of/Li is 4.1V so that the specific energy of lithium manganese phosphate material is higher, but the electric conductivity extreme difference of lithium manganese phosphate, limitation
Its development and application.
Iron manganese phosphate for lithium combines the advantage of above two material, both with 4V level capacities, and with good electric conductivity.
Due to the high-energy-density and other advantages of iron manganese phosphate lithium material, just the potential application material as electrokinetic cell of new generation.
The invention discloses a kind of preparation method of iron manganese phosphate lithium material, the iron manganese phosphate with good electrical property can be prepared
Lithium material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of iron manganese phosphate lithium material, iron manganese phosphate is synthesized first, so
The mixture with lithium dihydrogen phosphate and lithium carbonate reacts afterwards.Plus be spray-dried after carbonaceous organic material mixed grinding, powder after drying
Sintered under the atmosphere such as nitrogen, obtain iron manganese phosphate lithium material.
The present invention realizes that the technical scheme of purpose is：
A kind of iron manganese phosphate for lithium material preparation method, its preparation process is：
(1) analytically pure phosphoric acid Asia manganese, ferrous phosphate, lithium dihydrogen phosphate and lithium carbonate in molar ratio (0.8~0.9):
(0.2~0.1): 1: 1 ratio is added in hydrothermal reaction kettle, adds deionized water dissolving；
(2) reactor is heated into 180 DEG C to be kept for 12 hours, is then cooled to room temperature, take out whole materials, 105 DEG C of drums
Air-dry dry as bulk；
(3) 5% carbonaceous organic material and appropriate absolute ethyl alcohol are added in block, mixed sand is milled to 100~300nm, takes
Go out, be then spray-dried, as 2~10 μm or so particles.
(4) particle is sintered under the inert atmospheres such as nitrogen, 700 DEG C~800 DEG C is warmed up to the speed of 5 DEG C/min, protected
Hold 5 hours, be naturally cooling to room temperature, take out, obtain iron manganese phosphate for lithium.
Described carbonaceous organic material is one or two the mixture in glucose, PVA.
Specific embodiment
With reference to embodiment, the present invention is further described, and following embodiments are illustrative, be not it is limited,
Protection scope of the present invention can not be limited with following embodiments.
Embodiment 1
(1) 165.17g Mn3(PO4)2·3H2O (Tianjin good fortune morning chemical reagent factory, purity 99%), 50.67g Fe3
(PO4)2·8H2O (containing chemical reagent factory difficult to understand, purity 99% in Tianjin), 52.49g LiH2PO4、37.32g Li2CO3(upper marine lithium
Industrial Co., Ltd., purity 99%) add hydrothermal reaction kettle in, add 1000g deionized water dissolvings；
(2) reactor is heated into 180 DEG C to be kept for 12 hours, is then cooled to room temperature, take out whole materials, 105 DEG C of drums
Air-dry dry as bulk；
(3) 12g DEXTROSE ANHYDROUSs and 200ml absolute ethyl alcohols are added in block, mixed sand is milled to 100~300nm, takes
Go out, be then spray-dried, as 2~10 μm or so particles.
(4) particle is sintered under high pure nitrogen, 700 DEG C~800 DEG C is warmed up to the speed of 5 DEG C/min, holding 5 is small
When, room temperature is naturally cooling to, take out, obtain iron manganese phosphate for lithium.
Test prepare iron manganese phosphate lithium material, with lithium metal as negative pole, the material under 0.1C discharge-rates, gram volume
It is 158mAh/g.
Embodiment 2
(1) 185.82g Mn3(PO4)2·3H2O (Tianjin good fortune morning chemical reagent factory, purity 99%), 25.35g Fe3
(PO4)2·8H2O (containing chemical reagent factory difficult to understand, purity 99% in Tianjin), 52.49g LiH2PO4、37.32g Li2CO3(upper marine lithium
Industrial Co., Ltd., purity 99%) add hydrothermal reaction kettle in, add 1100g deionized water dissolvings；
(2) reactor is heated into 180 DEG C to be kept for 12 hours, is then cooled to room temperature, take out whole materials, 105 DEG C of drums
Air-dry dry as bulk；
(3) 6g PVA and 200ml absolute ethyl alcohols are added in block, mixed sand is milled to 100~300nm, is taken out, then
Spray drying, as 2~10 μm or so particles.
(4) particle is sintered under high pure nitrogen, 700 DEG C~800 DEG C is warmed up to the speed of 5 DEG C/min, holding 5 is small
When, room temperature is naturally cooling to, take out, obtain iron manganese phosphate for lithium.
Test prepare iron manganese phosphate lithium material, with lithium metal as negative pole, the material under 0.1C discharge-rates, gram volume
It is 160mAh/g.
Claims (2)
1. a kind of preparation method of iron manganese phosphate lithium material, it is characterised in that its preparation methods steps are：
(1) analytically pure phosphoric acid Asia manganese, ferrous phosphate, lithium dihydrogen phosphate, lithium carbonate in molar ratio (0.8~0.9): (0.2~
0.1): 1: 1 ratio is added in hydrothermal reaction kettle, deionized water dissolving is added；
(2) reactor is heated into 180 DEG C to be kept for 12 hours, is then cooled to room temperature, take out whole materials, 105 DEG C of air blast are done
It is dry as bulk；
(3) 5% carbonaceous organic material and appropriate absolute ethyl alcohol are added in block, mixed sand is milled to 100~300nm, is taken out, so
After be spray-dried, as 2~10 μm or so particles.
(4) particle is sintered under the atmosphere such as nitrogen, 700 DEG C~800 DEG C is warmed up to the speed of 5 DEG C/min, kept for 5 hours,
Room temperature is naturally cooling to, is taken out, obtain iron manganese phosphate for lithium.
2. the preparation method of a kind of iron manganese phosphate lithium material according to claim 1, it is characterised in that described carbon containing have
Machine thing is one or two the mixture in glucose, PVA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611062080.9A CN106784813A (en) | 2016-11-19 | 2016-11-19 | A kind of preparation method of iron manganese phosphate lithium material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611062080.9A CN106784813A (en) | 2016-11-19 | 2016-11-19 | A kind of preparation method of iron manganese phosphate lithium material |
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| Publication Number | Publication Date |
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| CN106784813A true CN106784813A (en) | 2017-05-31 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611062080.9A Pending CN106784813A (en) | 2016-11-19 | 2016-11-19 | A kind of preparation method of iron manganese phosphate lithium material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128892A (en) * | 2017-06-12 | 2017-09-05 | 百川化工(如皋)有限公司 | A kind of preparation method of lithium iron manganese phosphate anode material |
| CN108408709A (en) * | 2018-03-30 | 2018-08-17 | 南阳逢源锂电池材料研究所 | A kind of preparation process of pollution-free inexpensive iron manganese phosphate for lithium crystalline material |
| CN113078319A (en) * | 2021-03-26 | 2021-07-06 | 天津斯科兰德科技有限公司 | Preparation method of lithium iron manganese phosphate/carbon composite nanoparticle positive electrode material |
| CN115159491A (en) * | 2022-08-05 | 2022-10-11 | 湖北融通高科先进材料有限公司 | Preparation method of high-safety high-capacity lithium iron manganese phosphate |
| CN116332147A (en) * | 2023-03-29 | 2023-06-27 | 贵州安达科技能源股份有限公司 | Lithium manganese iron phosphate positive electrode material, preparation method and application thereof, and lithium ion battery |
| CN117613249A (en) * | 2024-01-22 | 2024-02-27 | 成都融捷锂业科技有限公司 | Composite electrode material and preparation method thereof |
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| CN102249208A (en) * | 2011-05-06 | 2011-11-23 | 朱鸥鹭 | Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery |
| CN103762362A (en) * | 2014-01-27 | 2014-04-30 | 厦门钨业股份有限公司 | Hydrothermal preparation method of nano lithium iron manganese phosphate anode material |
| CN104852037A (en) * | 2014-02-18 | 2015-08-19 | 北京有色金属研究总院 | Precursor rich in iron on surface and rich in manganese on core and method for preparing carbon-coated manganese-iron-lithium phosphate material by taking precursor as raw material |
| CN105552340A (en) * | 2016-02-01 | 2016-05-04 | 浙江天能能源科技有限公司 | Cathode material for lithium-ion battery and preparation method of cathode material |
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2016
- 2016-11-19 CN CN201611062080.9A patent/CN106784813A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249208A (en) * | 2011-05-06 | 2011-11-23 | 朱鸥鹭 | Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery |
| CN103762362A (en) * | 2014-01-27 | 2014-04-30 | 厦门钨业股份有限公司 | Hydrothermal preparation method of nano lithium iron manganese phosphate anode material |
| CN104852037A (en) * | 2014-02-18 | 2015-08-19 | 北京有色金属研究总院 | Precursor rich in iron on surface and rich in manganese on core and method for preparing carbon-coated manganese-iron-lithium phosphate material by taking precursor as raw material |
| CN105552340A (en) * | 2016-02-01 | 2016-05-04 | 浙江天能能源科技有限公司 | Cathode material for lithium-ion battery and preparation method of cathode material |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128892A (en) * | 2017-06-12 | 2017-09-05 | 百川化工(如皋)有限公司 | A kind of preparation method of lithium iron manganese phosphate anode material |
| CN108408709A (en) * | 2018-03-30 | 2018-08-17 | 南阳逢源锂电池材料研究所 | A kind of preparation process of pollution-free inexpensive iron manganese phosphate for lithium crystalline material |
| CN113078319A (en) * | 2021-03-26 | 2021-07-06 | 天津斯科兰德科技有限公司 | Preparation method of lithium iron manganese phosphate/carbon composite nanoparticle positive electrode material |
| CN115159491A (en) * | 2022-08-05 | 2022-10-11 | 湖北融通高科先进材料有限公司 | Preparation method of high-safety high-capacity lithium iron manganese phosphate |
| CN116332147A (en) * | 2023-03-29 | 2023-06-27 | 贵州安达科技能源股份有限公司 | Lithium manganese iron phosphate positive electrode material, preparation method and application thereof, and lithium ion battery |
| CN117613249A (en) * | 2024-01-22 | 2024-02-27 | 成都融捷锂业科技有限公司 | Composite electrode material and preparation method thereof |
| CN117613249B (en) * | 2024-01-22 | 2024-04-16 | 成都融捷锂业科技有限公司 | Composite electrode material and preparation method thereof |
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Application publication date: 20170531 |