CN106744774A - A kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate - Google Patents
A kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate Download PDFInfo
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- CN106744774A CN106744774A CN201710059124.0A CN201710059124A CN106744774A CN 106744774 A CN106744774 A CN 106744774A CN 201710059124 A CN201710059124 A CN 201710059124A CN 106744774 A CN106744774 A CN 106744774A
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- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 74
- 239000005955 Ferric phosphate Substances 0.000 title claims abstract description 58
- 229940032958 ferric phosphate Drugs 0.000 title claims abstract description 58
- 229910000399 iron(III) phosphate Inorganic materials 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 17
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 28
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 229910000398 iron phosphate Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000012141 concentrate Substances 0.000 claims abstract description 10
- 238000001556 precipitation Methods 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 150000002505 iron Chemical class 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 claims abstract description 3
- 210000004483 pasc Anatomy 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 34
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 230000006698 induction Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 abstract description 8
- 210000004027 cell Anatomy 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 5
- 238000003836 solid-state method Methods 0.000 description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 4
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910012820 LiCoO Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- QSNQXZYQEIKDPU-UHFFFAOYSA-N [Li].[Fe] Chemical compound [Li].[Fe] QSNQXZYQEIKDPU-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
- 229910021655 trace metal ion Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- 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
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Primary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The present invention provides a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate, and it includes that concentrate solution will be formed after phosphoric acid solution and the reaction of trivalent iron salt Hybrid Heating；Nano silicon and deionized water between above-mentioned concentrate to be added 1-3mol/L salpeter solutions and weight/mass percentage composition within the temperature range of 75 DEG C-85 DEG C for 0.01-0.1%, form iron phosphate crystal Precipitation is induced by nucleus of nano silicon, by being filtered, washed and dried, battery-grade iron phosphate material is prepared；The above-mentioned ferric phosphate for preparing is soaked into 20min to 60min in hydrofluoric acid, is washed out, dried, due to hydrofluoric acid and nano-silica pasc reaction so that the ferric phosphate product of above-mentioned preparation generates corrasion, finally prepares micropore spherical ferric phosphate material.Further to improve the follow-up electric conductivity and charge-discharge performance for preparing LiFePO4.The invention belongs to ferric phosphate preparing technical field.
Description
Technical field
The invention belongs to ferric phosphate preparation field, and in particular to a kind of method for preparing ferric phosphate.
Background technology
LiFePO4 due to theoretical capacity high (170mAh/g), high working voltage (voltage platform of 3.5V or so),
The premium properties such as good cycle, memory-less effect, and have the advantages that it is inexpensive, environment-friendly, therefore with substitution cost compared with
LiCoO high2And turn into anode material for lithium-ion batteries of new generation, and turned into the required large-scale energy-storage battery such as electric automobile
Important materials.Solid reaction process is widely used method in current LiFePO4 production and research process, and ferric phosphate is gradually
As the important presoma that LiFePO4 is made in carbothermic method.In CN 101337666A, CN 15181537A, CN
Source of iron is provided in the patent applications such as 1635648A, CN 101559935A, CN 101559935A with ferric phosphate and phosphorus source makes
The battery-grade iron phosphate lithium of function admirable.
But it is more by ferric phosphate impurities prepared by current method, the follow-up electric conductivity for preparing LiFePO4 of influence and
Charge-discharge performance, and preparation technology is complicated, it is relatively costly.Pertinent literature and experimental study show that the preparation of ferric phosphate is generally used
Trivalent iron salt mixes with phosphoric acid or soluble phosphoric acid salting liquid, using ammoniacal liquor or alkali lye control ph 1.8 or so, on 85 DEG C of left sides
Crystallization is formed under right heating condition；Ferric phosphate also can constitute mixed solution with divalent iron salt with phosphoric acid or soluble phosphate, lead to
Peroxide agent controls reaction condition with alkali lye, obtains form iron phosphate crystal.The ferric phosphate prepared is further prepared into LITHIUM BATTERY phosphorus
Sour iron lithium.The chemical property of the pattern of ferric phosphate presoma, purity and trace metal ion content to follow-up LiFePO4
Have a major impact.
The content of the invention
It is an object of the invention to：A kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate is provided, further to improve
The follow-up electric conductivity and charge-discharge performance for preparing LiFePO4.
To solve the above problems, there is provided a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate, comprise the following steps：
Phosphoric acid solution and trivalent iron salt are 6 according to P elements and ferro element mol ratio by step 1.：1 mixed dissolution, mixing
Afterwards, phosphate radical molar concentration control between 0.3-1.2mol/L, molysite molar concentration control 0.05-0.2mol/L it
Between, concentrate solution is formed after heating response；
Step 2：Above-mentioned concentrate is added into salpeter solution and nano silicon within the temperature range of 75 DEG C -85 DEG C
And deionized water, form iron phosphate crystal Precipitation is induced by nucleus of nano silicon, by being filtered, washed and dried,
Prepare battery-grade iron phosphate material；
Step 3：20min to 60min is soaked during the above-mentioned ferric phosphate for preparing is added into hydrofluoric acid solution, phosphoric acid is added
After iron, the weight/mass percentage composition of hydrofluoric acid is 0.5% -5%, is washed out, dries, hydrofluoric acid and nano-silica pasc reaction, is made
The ferric phosphate product for obtaining above-mentioned preparation produces corrasion, finally prepares micropore spherical ferric phosphate material.
Trivalent iron salt described in step 1 is ferric trichloride or ferric nitrate, and described concentrate solution refers to be by content
85% concentrated phosphoric acid, trivalent iron salt and deionized water, are 6 by ferrophosphorus elemental mole ratios：After 1 is configured to mixed solution,
At a temperature of 90-100 DEG C, agitating heating is concentrated into the 30%-50% of original solution volume；
In step 2, after adding salpeter solution, nano silicon and deionized water so that after mixing in solution, nitric acid
Molar concentration be 1-3mol/L, the weight/mass percentage composition of nano silicon is 0.01-0.1%, iron concentration control
Between 0.05-3mol/L, described induction ferric phosphate Precipitation refers to addition nano silicon and nitre in concentrate solution
After acid, the constant temperature stirring 1-3h between 75 DEG C of -85 DEG C of temperature ranges, nano silicon and nitric acid are to micro-chemical environment around
Generation influence so that the ferric phosphate in mixed solution is nucleus Precipitation with nano silicon, will be precipitated after reaction fully
Filtering, is washed to precipitation, is dried, is prepared D50Granularity the ferric phosphate of 0.1-3 μ ms process, described nanoscale
More than 99.5%, granularity is in the range of 15-30nm for the purity requirement of silica.
Compared with prior art, due to using raw material type few, the ferric phosphate impurity content prepared is few, ball-type for the present invention
Ferric phosphate contains abundant nanoporous structure, even particle size distribution, it is adaptable to further prepare the electricity of excellent electrochemical performance
Pond level LiFePO4；Technical process is simple, and technological parameter controllability is strong, wide material sources few using raw material type, low cost, fits
Technical scale metaplasia is closed to produce.
Brief description of the drawings
Fig. 1 is ferric phosphate spherome surface microscopic appearance figure；
Fig. 2 is ferric phosphate ball interior microscopic appearance figure.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, will make further detailed to the present invention below
Description,
Embodiment 1：
Step 1：Measure 15molL-1Phosphoric acid solution 21.00ml, add FeCl3·6H2O14.00g, and 200ml
Deionized water, agitating heating 90 minutes under the conditions of 100 DEG C are concentrated into volume for 100ml.
Step 2：After above-mentioned solution is slightly cold, it is 65% -68% concentrated nitric acid to add 40ml contents, adds 0.32g nanometers two
Silica, 1L is diluted to deionized water, and under 80 DEG C of temperature conditionss, constant temperature stirring 3h, with nano silicon as nucleus, draws
Ferric phosphate crystalline deposit is separated out in playing solution, is then filtered pelleting centrifugation, washs, is dried, and prepares battery-grade iron phosphate.
Step 3：The ferric phosphate of above-mentioned preparation is put into the hydrofluoric acid that 100ml concentration is 1% and is soaked 40 minutes, use middling speed
Quantitative filter paper is filtered, and is washed out, is dried, and prepares micropore global cell level iron phosphate material.
High temperature solid-state method is reduced with charcoal further prepare ferric phosphate lithium cell level material, the first charge-discharge under 0.1C multiplying powers
Performance reaches 160mAh/g.
Embodiment 2：
Step 1：Measure 15molL-1Phosphoric acid solution 21.00ml, add FeCl36H2O14.00g, and
200.00ml deionized waters, agitating heating 90 minutes under the conditions of 100 DEG C are concentrated into volume for 100ml.
Step 2：After above-mentioned solution is slightly cold, add 20ml contents for 65% -68% nitric acid and 0.32g nanometer titanium dioxides
Silicon, deionized water is diluted to 1L, when under the conditions of 75 DEG C, constant temperature stirring 3h, with nano silicon as nucleus, in causing solution
Ferric phosphate crystalline deposit is separated out, and is then filtered pelleting centrifugation, washs, is dried, and prepares battery-grade iron phosphate.
Step 3：The ferric phosphate of above-mentioned preparation is put into the hydrofluoric acid that 100ml concentration is 2% and is soaked 30 minutes, use middling speed
Quantitative filter paper is filtered, washing, is dried, and prepares micropore spherical ferric phosphate material.
High temperature solid-state method is reduced with charcoal further prepare ferric phosphate lithium cell level material, the first charge-discharge under 0.1C multiplying powers
Performance reaches 158mAh/g.
Embodiment 3：
Step 1：Measure 15molL-1Phosphoric acid solution 25.00ml, add FeCl3·6H2O15.00g, and 200ml
Deionized water, agitating heating 120 minutes under the conditions of 100 DEG C are concentrated into volume for 80ml.
Step 2：After above-mentioned solution is slightly cold, it is 65% -68% concentrated nitric acid to add 30ml contents, adds 0.32g nanometers two
Silica, 1L is diluted to deionized water, and under 80 DEG C of temperature conditionss, constant temperature stirring 2h, with nano silicon as nucleus, draws
Ferric phosphate crystalline deposit is separated out in playing solution, is then filtered pelleting centrifugation, washs, is dried, and prepares battery-grade iron phosphate.
Step 3：The ferric phosphate of above-mentioned preparation is put into the hydrofluoric acid that 100ml concentration is 3% and is soaked 30 minutes, use middling speed
Quantitative filter paper is filtered, and is washed out, is dried, and prepares micropore global cell level iron phosphate material.
High temperature solid-state method is reduced with charcoal further prepare ferric phosphate lithium cell level material, the first charge-discharge under 0.1C multiplying powers
Performance reaches 165mAh/g.
Embodiment 4：
Step 1：Measure 15molL-1Phosphoric acid solution 21.00ml, add FeCl3·6H2O14.00g, and 200ml
Deionized water, agitating heating 90 minutes under the conditions of 100 DEG C are concentrated into volume for 60ml.
Step 2：After above-mentioned solution is slightly cold, it is 65% -68% concentrated nitric acid to add 20ml contents, adds 0.32g nanometers two
Silica, 1L is diluted to deionized water, and under 80 DEG C of temperature conditionss, constant temperature stirring 2h, with nano silicon as nucleus, draws
Ferric phosphate crystalline deposit is separated out in playing solution, is then filtered pelleting centrifugation, washs, is dried, and prepares battery-grade iron phosphate.
Step 3：The ferric phosphate of above-mentioned preparation is put into the hydrofluoric acid that 100ml concentration is 2% and is soaked 40 minutes, use middling speed
Quantitative filter paper is filtered, and is washed out, is dried, and prepares micropore global cell level iron phosphate material.
High temperature solid-state method is reduced with charcoal further prepare ferric phosphate lithium cell level material, the first charge-discharge under 0.1C multiplying powers
Performance reaches 153mAh/g.
Embodiment 5：
Step 1：Measure 15molL-1Phosphoric acid solution 21.00ml, add FeCl3·6H2O14.00g, and 200ml
Deionized water, agitating heating 120 minutes under the conditions of 100 DEG C are concentrated into volume for 60ml.
Step 2：After above-mentioned solution is slightly cold, it is 65% -68% concentrated nitric acid to add 20ml contents, adds 0.32g nanometers two
Silica, 1L is diluted to deionized water, under 85 DEG C of temperature conditionss, constant temperature stirring 1.5h, and with nano silicon as nucleus,
Ferric phosphate crystalline deposit is separated out in causing solution, is then filtered pelleting centrifugation, washs, is dried, and prepares battery-grade iron phosphate.
Step 3：The ferric phosphate of above-mentioned preparation is put into the hydrofluoric acid that 100ml concentration is 2% and is soaked 40 minutes, use middling speed
Quantitative filter paper is filtered, and is washed out, is dried, and prepares micropore global cell level iron phosphate material.
High temperature solid-state method is reduced with charcoal further prepare ferric phosphate lithium cell level material, the first charge-discharge under 0.1C multiplying powers
Performance reaches 162mAh/g.
The microscopic appearance of ferric phosphate is shown in Fig. 1 and Fig. 2 prepared by embodiment 5.
Claims (6)
1. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate, it is characterised in that comprise the following steps：
Phosphoric acid solution and trivalent iron salt are 6 according to P elements and ferro element mol ratio by step 1.：1 mixed dissolution, after mixing, phosphorus
Acid group molar concentration is controlled between 0.3-1.2mol/L, and molysite molar concentration is controlled between 0.05-0.2mol/L, heating
Concentrate solution is formed after reaction；
Step 2：Within the temperature range of 75 DEG C -85 DEG C by above-mentioned concentrate add salpeter solution and nano silicon and
Deionized water, form iron phosphate crystal Precipitation is induced by nucleus of nano silicon, by being filtered, washed and dried, is prepared
Go out battery-grade iron phosphate material；
Step 3：20min to 60min is soaked during the above-mentioned ferric phosphate for preparing is added into hydrofluoric acid solution, ferric phosphate is added
Afterwards, the weight/mass percentage composition of hydrofluoric acid is 0.5% -5%, is washed out, dries, hydrofluoric acid and nano-silica pasc reaction so that
The ferric phosphate product of above-mentioned preparation produces corrasion, finally prepares micropore spherical ferric phosphate material.
2. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate according to claim 1, it is characterised in that：In step 1
Described trivalent iron salt is ferric trichloride or ferric nitrate.
3. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate according to claim 1, it is characterised in that：In step 1
Described concentrate solution refers to by concentrated phosphoric acid, trivalent iron salt and deionized water that content is 85%, by ferrophosphorus element mole
Than being 6：After 1 is configured to mixed solution, at a temperature of 90-100 DEG C, agitating heating is concentrated into the 30%- of original solution volume
50%.
4. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate according to claim 1, it is characterised in that：In step 2,
After adding salpeter solution, nano silicon and deionized water so that after mixing in solution, the molar concentration of nitric acid for 1-
3mol/L, the weight/mass percentage composition of nano silicon is 0.01-0.1%, iron concentration control 0.05-3mol/L it
Between.
5. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate according to claim 1, it is characterised in that：In step 2
Described induction ferric phosphate Precipitation refers to after adding nano silicon and nitric acid in concentrate solution, in 75 DEG C of -85 DEG C of temperature
Constant temperature stirring 1-3h between degree scope, nano silicon and nitric acid produce influence to micro-chemical environment around so that mixing is molten
Ferric phosphate in liquid is nucleus Precipitation with nano silicon, filters precipitation after reaction fully, precipitation is washed,
Dry, prepare D50Process of the granularity in the ferric phosphate of 0.1-3 μ ms.
6. a kind of preparation method of LITHIUM BATTERY micropore spherical ferric phosphate according to claim 1, it is characterised in that：In step 2
More than 99.5%, granularity is in the range of 15-30nm for the purity requirement of described nanometer grade silica.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439361A (en) * | 2018-04-09 | 2018-08-24 | 杭州电子科技大学 | A kind of preparation method of spherical nano ferric phosphate |
| CN108767197A (en) * | 2018-06-05 | 2018-11-06 | 贵州大学 | A kind of preparation method of optimization based lithium-ion battery positive plate |
| CN109065877A (en) * | 2018-10-09 | 2018-12-21 | 湖南雅城新材料有限公司 | A kind of preparation method of nanoscale iron phosphate |
| CN110642235A (en) * | 2019-10-25 | 2020-01-03 | 湖北万润新能源科技发展有限公司 | Preparation method of core-shell structure battery-grade anhydrous iron phosphate |
| CN111029571A (en) * | 2019-11-22 | 2020-04-17 | 贵州唯特高新能源科技有限公司 | Preparation method of silicon dioxide uniformly doped iron phosphate |
| CN111017899A (en) * | 2019-10-29 | 2020-04-17 | 李冬 | Iron phosphate with nano-microporous structure and preparation method thereof |
| CN111362243A (en) * | 2020-05-27 | 2020-07-03 | 湖南雅城新材料有限公司 | Preparation method of iron phosphate for lithium battery |
| CN115465846A (en) * | 2022-09-13 | 2022-12-13 | 宜都兴发化工有限公司 | Preparation method of porous iron phosphate |
| CN116924376A (en) * | 2023-09-18 | 2023-10-24 | 贝特瑞（天津）纳米材料制造有限公司 | Method for preparing high-compaction and high-conductivity lithium iron phosphate based on bimodal particle size ferric phosphate |
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| CN102476793A (en) * | 2010-11-23 | 2012-05-30 | 贵州大学 | Sol method for preparing electronic-grade ferric phosphate |
| US9133029B2 (en) * | 2012-09-13 | 2015-09-15 | Tsinghua University | Method for making lithium iron phosphate cathode material |
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| CN102476793A (en) * | 2010-11-23 | 2012-05-30 | 贵州大学 | Sol method for preparing electronic-grade ferric phosphate |
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