CN115285958A - Preparation method of battery-grade iron phosphate - Google Patents
Preparation method of battery-grade iron phosphate Download PDFInfo
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- CN115285958A CN115285958A CN202210079702.8A CN202210079702A CN115285958A CN 115285958 A CN115285958 A CN 115285958A CN 202210079702 A CN202210079702 A CN 202210079702A CN 115285958 A CN115285958 A CN 115285958A
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- phosphate
- iron
- iron phosphate
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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 43
- 229910000398 iron phosphate Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 17
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011574 phosphorus Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 150000002505 iron Chemical class 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 7
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 5
- -1 iron ions Chemical class 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000404 tripotassium phosphate Inorganic materials 0.000 claims description 2
- 235000019798 tripotassium phosphate Nutrition 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 2
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 12
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 4
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 4
- 239000005955 Ferric phosphate Substances 0.000 description 3
- 229940032958 ferric phosphate Drugs 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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
- C01P2006/80—Compositional purity
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of battery-grade iron phosphate, which comprises the following specific steps: s1, preparing an iron salt solution, dissolving an iron source in pure water to prepare the iron salt solution, and adding a surfactant; s2, preparing a phosphorus source solution, dissolving a phosphorus source in pure water, and uniformly stirring to prepare the phosphorus source solution; s3, carrying out oxidation precipitation reaction, namely adding an iron salt solution into a reaction kettle, heating the reaction kettle, adding a phosphorus source solution, continuously stirring to uniformly mix feed liquid, standing after the reaction is finished, and discharging the feed liquid; and S4, filtering, washing and drying the feed liquid discharged in the step S3 to obtain an iron phosphate product. The iron phosphate product obtained by the invention meets the technical index of battery-grade iron phosphate, the particle size of the iron phosphate product is about 50nm, the particle size of the product is uniform, and the purity is high.
Description
Technical Field
The invention relates to the technical field of iron phosphate preparation processes, in particular to a preparation method of battery-grade iron phosphate.
Background
In recent years, with the rapid development of new energy industries, lithium batteries are more and more widely applied in the traffic field, and are mainly used as auxiliary standby power supplies, standby power traction sources and power supplies of vehicles. Iron phosphate (FePO) 4 ·nH 2 O, n = 0-2), also known as ferric orthophosphate or ferric phosphate, is generally white or yellowish white powder, and is a main precursor for preparing lithium iron phosphate as a positive electrode material of a lithium battery. The product performance of the iron phosphate is important for preparing the lithium iron phosphate of the battery anode, and the particle size and uniformity of the iron phosphate directly influence the particle size and uniformity of the prepared lithium iron phosphate and finally influence the electrochemical performance of the whole battery. At present, a plurality of manufacturers for producing battery grade iron phosphate at home and abroad exist, and the product performance is uneven due to different production processes and quality control standards of all the manufacturers. Chinese patent CN202011279498.1 introduces a nano-scale iron phosphate precursor and a preparation method thereof, and lithium iron phosphate and a preparation method thereof, wherein NH is used 4 H 2 PO 4 、FeCl 3 The ferric phosphate product is prepared by taking furfuryl alcohol and ammonia water as raw materials. The preparation process is complex to operate, the reaction time is long, and the obtained product is poor in uniformity. Chinese patent CN107565132B introduces a preparation method of iron phosphate and the prepared iron phosphate, which takes sulfuric acid, organic acid, reduced iron powder, ammonium persulfate, ammonium phosphate and nano particle control agent as raw materials, and the iron phosphate product is prepared after reaction for 5-8 h. The method has the advantages of complex raw materials and long reaction time, and the obtained iron phosphate has uneven particle size. Therefore, the development of a preparation method of battery grade iron phosphate with simple preparation process and uniform particle size of the obtained product is an urgent problem to be solved in the field.
Disclosure of Invention
In view of this, the invention provides a preparation method of battery grade iron phosphate, which can obtain a battery grade iron phosphate product with higher purity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of battery-grade iron phosphate comprises the following specific steps:
s1, preparing an iron salt solution, dissolving an iron source in pure water to prepare the iron salt solution, wherein the mass percentage concentration of iron ions in the solution is 10-13%, and adding a surfactant;
s2, preparing a phosphorus source solution, dissolving a phosphorus source in pure water, and uniformly stirring to prepare the phosphorus source solution, wherein the mass percentage concentration of phosphate radicals in the solution is 17-21%, and the phosphorus source is one of trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate;
s3, carrying out oxidation precipitation reaction, namely adding an iron salt solution into a reaction kettle, heating the reaction kettle through a temperature regulating device, adding a phosphorus source solution into the reaction kettle, continuously stirring to uniformly mix feed liquid, standing after the reaction is finished, and discharging the feed liquid;
and S4, filtering, washing and drying the feed liquid discharged in the step S3 to obtain an iron phosphate product.
Preferably, the surfactant in step S1 is cetyl trimethyl ammonium bromide, and the mass of the added surfactant is 1.5% of the mass of the iron salt.
Preferably, the molar ratio of the iron ions in the step S1 to the phosphate radicals in the step S2 is 0.95-1.30:1.
preferably, the stirring speed in step S2 is 300 to 500rpm.
Preferably, the retention time of the feed liquid in the step S3 in the reaction kettle is 40-50min.
Preferably, in the step S3, the temperature of the feed liquid in the reaction kettle is controlled to be 85-90 ℃.
The invention has the following beneficial effects:
according to the preparation method of the battery-grade nano iron phosphate, the iron phosphate product is prepared through an oxidation precipitation reaction. The pH is not required to be adjusted in the preparation process, the reaction temperature is only required to reach 85-90 ℃, the preparation process is simple, and the cost is low. The obtained iron phosphate product meets the technical index of battery-grade iron phosphate, the particle size of the iron phosphate product is about 50nm, the particle size of the product is uniform, and the purity is high.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a microscopic topography of the nano iron phosphate prepared in example 1.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment 1 of the invention discloses a preparation method of battery-grade iron phosphate.
Experimental reagents and materials: ferric trichloride, analytically pure; disodium hydrogen phosphate, analytically pure; hexadecyl trimethyl ammonium bromide, analytically pure.
Preparation of iron salt solution:
weighing 2.7g of ferric trichloride particles, adding into a beaker, adding a proper amount of deionized water, stirring for dissolving, fixing the volume to 25ml, and standing for later use, wherein the mass percent concentration of iron ions in the solution is 10.8%.
Preparing a phosphorus source solution:
weighing 4.65g of disodium hydrogen phosphate particles according to the iron-phosphorus molar ratio, placing the disodium hydrogen phosphate particles in a beaker, adding water, stirring and dissolving, fixing the volume to 25ml, and standing for later use, wherein the mass percent concentration of phosphate radicals in the solution is 18.6%.
Preparing iron phosphate:
adding a ferric salt solution into a reaction kettle, heating the reaction kettle to 85-90 ℃ through a temperature regulating device, slowly adding a phosphorus source solution into the reaction kettle, wherein the feeding time is about 10min, continuously stirring for 15-20min to uniformly mix and fully react the feed liquid, discharging the feed liquid after the reaction is finished, and filtering, washing and drying the discharged feed liquid to finally obtain the ferric phosphate product.
Sample analysis
According to the related technical requirements on preparation of the iron phosphate for the battery in the chemical industry standard of the people's republic of China (HG/T4701-2014), detection and analysis are mainly carried out according to the appearance of a sample and the content of related main elements. The results are as follows:
appearance of the sample: nearly white powder, uniform particle size.
The element content is as follows: and (3) determining the contents of three main elements of Fe, P and Cl according to the used reagent, wherein the contents of Fe and P are determined by adopting an ICP-OES method, the content of Cl is determined by adopting a silver nitrate titration method, and the comparison result of the content of the sample element and the standard index is shown in a table 1. As can be seen from Table 1, the chloride content of the three groups of samples is 0.01%, which meets the standard, when the molar ratio of phosphorus to iron is 1:1, the Fe content of the obtained sample is 29.27 percent, the P content is 16.78 percent, and the iron-phosphorus ratio is 0.97, which meets the standard.
TABLE 1 comparison of sample element content with Standard index
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. The preparation method of the battery grade iron phosphate is characterized by comprising the following specific steps:
s1, preparing an iron salt solution, dissolving an iron source in pure water to prepare the iron salt solution, wherein the mass percentage concentration of iron ions in the solution is 10-13%, and adding a surfactant;
s2, preparing a phosphorus source solution, dissolving a phosphorus source in pure water, and uniformly stirring to prepare the phosphorus source solution, wherein the mass percentage concentration of phosphate radicals in the solution is 17-21%, and the phosphorus source is one of trisodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, tripotassium phosphate, dipotassium hydrogen phosphate and potassium dihydrogen phosphate;
s3, carrying out oxidation precipitation reaction, namely adding an iron salt solution into a reaction kettle, heating the reaction kettle through a temperature regulating device, adding a phosphorus source solution into the reaction kettle, continuously stirring to uniformly mix feed liquid, standing after the reaction is finished, and discharging the feed liquid;
and S4, filtering, washing and drying the feed liquid discharged in the step S3 to obtain an iron phosphate product.
2. The method for preparing battery grade iron phosphate according to claim 1, wherein the surfactant in step S1 is cetyl trimethyl ammonium bromide, and the mass of the added surfactant is 1.5% of the mass of the iron salt.
3. The method for preparing battery grade iron phosphate according to claim 1, wherein the molar ratio of the iron ions in the step S1 to the phosphate in the step S2 is 0.95-1.30:1.
4. the method for preparing battery grade iron phosphate according to claim 1, wherein the stirring speed in the step S2 is 300-500rpm.
5. The method for preparing battery grade iron phosphate according to claim 1, wherein the retention time of the feed liquid in the step S3 in the reaction kettle is 40-50min.
6. The method for preparing battery grade iron phosphate according to claim 1, wherein in the step S3, the temperature of the feed liquid in the reaction kettle is controlled to be 85-90 ℃.
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| CN108117055A (en) * | 2017-12-30 | 2018-06-05 | 彩客化学（东光）有限公司 | The preparation method and process units of a kind of battery-grade iron phosphate |
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