CN115140721A - Method for synthesizing battery-grade iron phosphate from byproduct ferrous sulfate and byproduct phosphoric acid - Google Patents
Method for synthesizing battery-grade iron phosphate from byproduct ferrous sulfate and byproduct phosphoric acid Download PDFInfo
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- CN115140721A CN115140721A CN202210569721.9A CN202210569721A CN115140721A CN 115140721 A CN115140721 A CN 115140721A CN 202210569721 A CN202210569721 A CN 202210569721A CN 115140721 A CN115140721 A CN 115140721A
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- ferrous sulfate
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- byproduct
- iron phosphate
- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 112
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 107
- 239000006227 byproduct Substances 0.000 title claims abstract description 96
- 229910000398 iron phosphate Inorganic materials 0.000 title claims abstract description 96
- 239000011790 ferrous sulphate Substances 0.000 title claims abstract description 85
- 235000003891 ferrous sulphate Nutrition 0.000 title claims abstract description 85
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 title claims abstract description 85
- 229910000359 iron(II) sulfate Inorganic materials 0.000 title claims abstract description 85
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 48
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 88
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 41
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 35
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 21
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 20
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 18
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 18
- CZPWVGJYEJSRLH-UHFFFAOYSA-N Pyrimidine Chemical compound C1=CN=CN=C1 CZPWVGJYEJSRLH-UHFFFAOYSA-N 0.000 claims abstract description 17
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 239000008394 flocculating agent Substances 0.000 claims abstract description 8
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims description 49
- 150000002500 ions Chemical class 0.000 claims description 31
- 235000010215 titanium dioxide Nutrition 0.000 claims description 21
- 239000004094 surface-active agent Substances 0.000 claims description 19
- 239000000047 product Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 8
- 229920000767 polyaniline Polymers 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 8
- 229910052742 iron Inorganic materials 0.000 abstract description 6
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 12
- 239000005955 Ferric phosphate Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 11
- 229940032958 ferric phosphate Drugs 0.000 description 11
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 235000019270 ammonium chloride Nutrition 0.000 description 8
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 8
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 8
- 235000019837 monoammonium phosphate Nutrition 0.000 description 8
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 8
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 7
- 235000011130 ammonium sulphate Nutrition 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 239000012047 saturated solution Substances 0.000 description 5
- -1 and meanwhile Substances 0.000 description 4
- 239000007788 liquid Substances 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
- 239000011572 manganese Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 229910001447 ferric ion Inorganic materials 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 3
- FOEMIZSFFWGXHX-UHFFFAOYSA-N 2-methylsulfanylpyrimidine Chemical compound CSC1=NC=CC=N1 FOEMIZSFFWGXHX-UHFFFAOYSA-N 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical group [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000006824 pyrimidine synthesis Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- XJPZKYIHCLDXST-UHFFFAOYSA-N 4,6-dichloropyrimidine Chemical compound ClC1=CC(Cl)=NC=N1 XJPZKYIHCLDXST-UHFFFAOYSA-N 0.000 description 1
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 description 1
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001308 synthesis method 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
-
- 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)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for synthesizing battery-grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid, which comprises the following steps: adding deionized water to dissolve ferrous sulfate as a titanium dioxide byproduct, and filtering to obtain a ferrous sulfate solution; adding a sodium sulfide solution into a ferrous sulfate solution, and filtering to obtain a filtrate; adding reduced iron powder into the filtrate, adjusting the pH value by adding ammonia water, adding a flocculating agent, and filtering to obtain a purified ferrous sulfate solution; mixing the purified ferrous sulfate solution with hydrogen peroxide and a pyrimidine by-product phosphoric acid solution to obtain a first mixed solution; mixing sodium hydroxide and ammonia water to obtain a second mixed solution; pumping the first mixed solution and the second mixed solution into a reaction kettle, heating and stirring, and performing suction filtration to obtain iron phosphate precipitate; and washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times to obtain the battery-grade iron phosphate. The invention can solve the technical problem of high cost of raw materials of iron source and phosphoric acid source in the prior art.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to a method for synthesizing battery-grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid.
Background
With the continuous development of lithium ion batteries, the positive electrode material of the lithium ion battery becomes a hotspot of research, and comprises lithium iron phosphate, lithium manganate, lithium nickel cobalt manganese oxide, lithium nickel cobalt aluminate and the like, wherein the lithium iron phosphate is developed rapidly in China with the advantages of higher safety stability, longer cycle life and lower cost, the iron source of the lithium iron phosphate is mostly ferric phosphate, and the purity of the ferric phosphate synthesis directly affects the performance of the lithium iron phosphate, so the synthesis of the ferric phosphate plays a crucial role in the lithium ion battery.
At present, a common method for synthesizing battery-grade iron phosphate generally adopts a method that raw material iron salt reacts with phosphate to generate iron phosphate, the process is simple and mature, however, the production cost of the raw material iron source and the phosphoric acid source is high, and the cost for synthesizing the iron phosphate is increased, so that the production cost of the lithium ion battery is increased.
Therefore, the existing method for synthesizing battery grade iron phosphate generally has the technical problem that the cost of the raw material iron source and the phosphoric acid source is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for synthesizing battery-grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid, and aims to solve the technical problem that the cost of raw material iron sources and phosphoric acid sources is high in the prior art.
One aspect of the present invention provides a method for synthesizing battery grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid, comprising:
adding deionized water into titanium dioxide byproduct ferrous sulfate for dissolving, and filtering to remove insoluble impurities to obtain a ferrous sulfate solution;
adding a sodium sulfide solution into the ferrous sulfate solution, stirring and filtering to obtain a filtrate;
adding reduced iron powder into the filtrate, adjusting the pH value to 3.5-4.5 by adding ammonia water, heating to 80-100 ℃, stirring for 1.5-2.5h, cooling, standing, adding a flocculating agent, and filtering to remove impurities to obtain a purified ferrous sulfate solution;
mixing the purified ferrous sulfate solution with hydrogen peroxide and a pyrimidine by-product phosphoric acid solution to obtain a first mixed solution;
mixing sodium hydroxide and ammonia water to obtain a second mixed solution;
adding a surfactant into deionized water for dissolving, adding into a reaction kettle, heating and stirring;
slowly pumping the first mixed solution and the second mixed solution into the reaction kettle through a first pump pipe and a second pump pipe respectively, heating to 80-100 ℃, stirring for 1.5-2.5h, and performing suction filtration to obtain iron phosphate precipitate;
and washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times to obtain the battery-grade iron phosphate.
Compared with the prior art, the invention has the beneficial effects that: according to the method for synthesizing the battery-grade iron phosphate by using the byproduct ferrous sulfate and the byproduct phosphoric acid, the battery-grade iron phosphate is prepared by using the byproduct ferrous sulfate of titanium white and the byproduct phosphoric acid of pyrimidine as raw materials, so that the recycling of the byproduct ferrous sulfate of titanium white and the byproduct phosphoric acid of pyrimidine is realized, the iron phosphate with high purity and small crystal grains is prepared, the requirements of the battery-grade iron phosphate are met, and the method is economical and environment-friendly.
According to one aspect of the above technical scheme, the step of washing, filtering and drying the iron phosphate precipitate with an ammonia water solution of a preset concentration for a preset number of times to obtain battery grade iron phosphate specifically comprises:
calculating by using different solubility products of different ions in the ammonia water solution according to a solubility product formula to obtain that impurity ions in the iron phosphate precipitate can be preferentially dissolved in the ammonia water solution with preset concentration;
and washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with a preset concentration for a preset number of times, and preferentially removing impurity ions to obtain the battery-grade iron phosphate.
According to one aspect of the above technical scheme, the preset concentration of the ammonia water solution is 0.05% -0.15%, and the preset times are 5-15%.
According to one aspect of the above technical scheme, the step of dissolving the titanium dioxide byproduct ferrous sulfate in deionized water, filtering to remove insoluble impurities to obtain a ferrous sulfate solution specifically comprises:
adding 75-95g of ferrous sulfate serving as a titanium white byproduct into 300-500ml of deionized water, and stirring for dissolving;
insoluble impurities in the solution were removed by filtration to obtain a ferrous sulfate solution.
According to one aspect of the above technical solution, the step of adding sodium sulfide to the ferrous sulfate solution, stirring and filtering to obtain a filtrate specifically includes:
dissolving sodium sulfide in deionized water to prepare 40-60ml of sodium sulfide solution with the concentration of 20-40 g/L;
and adding the sodium sulfide solution into the ferrous sulfate solution, stirring for 5-15min, and carrying out suction filtration to obtain a filtrate.
According to one aspect of the technical scheme, the method comprises the steps of adding reduced iron powder into the filtrate, adjusting the pH value to 3.5-4.5 by adding ammonia water, heating to 80-100 ℃, stirring for 1.5-2.5h, cooling, standing, adding a flocculating agent, filtering and removing impurities to obtain a purified ferrous sulfate solution, and specifically comprises the following steps:
heating the filtrate to 80-100 ℃ under the condition of stirring, adding 0.5-1.5g of reduced iron powder, adjusting the pH of the filtrate to 3.5-4.5 by adding ammonia water, and stirring for 1.5-2.5h;
standing and cooling after stirring, adding the polyaniline as flocculant, standing for 20-40min, and filtering to remove impurities to obtain a purified ferrous sulfate solution.
According to one aspect of the above technical scheme, the addition amount of the hydrogen peroxide is 20-30ml, the concentration of the pyrimidine by-product phosphoric acid solution is 30% -40%, and the addition amount is 80-100ml.
According to one aspect of the above technical scheme, the steps of adding the surfactant into deionized water for dissolution, adding into a reaction kettle, heating and stirring include:
adding surfactant with the mass of 0.5-1.5g into deionized water of 40-60ml for dissolving to prepare surfactant solution;
adding the surfactant solution into a reaction kettle, and heating to 80-100 ℃ under the condition of stirring.
According to one aspect of the above technical solution, the diameter of the first pump tube is 20-30mm, and the diameter of the second pump tube is 10-20mm.
According to one aspect of the above technical solution, the second mixed solution is pumped into the reaction kettle to control the pH of the reaction environment to be 1.5-2.3.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a flow chart illustrating a method for synthesizing battery-grade iron phosphate from by-product ferrous sulfate and by-product phosphoric acid according to a first embodiment of the present invention.
Detailed Description
In order to make the objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. Several embodiments of the invention are presented in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. As used herein, the terms "vertical," "horizontal," "left," "right," "up," "down," and the like are used for descriptive purposes only and not for purposes of indicating or implying that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.
In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," "fixed," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example one
Referring to fig. 1, a method for synthesizing battery-grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid according to the present invention is shown, the method includes steps S10 to S17:
step S10, adding deionized water to dissolve ferrous sulfate serving as a titanium dioxide byproduct, and filtering to remove insoluble impurities to obtain a ferrous sulfate solution;
at present, the domestic titanium dioxide is generally produced by adopting a sulfuric acid method, a large amount of by-product ferrous sulfate can be generated in the production process of titanium dioxide by the sulfuric acid method, most of the by-product ferrous sulfate is treated as waste products and is accumulated along with the ground, and serious pollution is caused to the environment.
The ferrous sulfate as a byproduct of titanium dioxide contains impurities, and cannot be directly used for synthesizing battery-grade iron phosphate, and the battery-grade iron phosphate is usually synthesized after purification.
Specifically, adding 75-95g of ferrous sulfate as a titanium white byproduct into 300-500ml of deionized water, and stirring for dissolving;
insoluble impurities in the solution were removed by filtration to obtain a ferrous sulfate solution.
Step S11, adding a sodium sulfide solution into the ferrous sulfate solution, stirring and filtering to obtain a filtrate;
wherein, the main impurity ion in the ferrous sulfate as the byproduct of titanium dioxide is Al 3+ 、Mn 2+ And Ti 4+ Therefore, the battery-grade iron phosphate can be synthesized only after the three elements are purified, so that the purity and the performance of the battery-grade iron phosphate are ensured to be good. Usually for impurity ions Al 3+ 、Mn 2+ And Ti 4+ Sulfide can be added to precipitate, sodium sulfide is used as precipitant to remove impurity ion Al 3+ 、Mn 2+ And Ti 4+ . Wherein, after addition of the sodium sulfide solution, mn 2+ The content of the titanium dioxide is reduced to be below 0.01 percent, the impurity removal effect is obvious, and the purification of the ferrous sulfate as a titanium dioxide byproduct is facilitated.
Specifically, sodium sulfide is dissolved in deionized water, and 40-60ml of sodium sulfide solution with the concentration of 20-40g/L is prepared;
adding the sodium sulfide solution into the ferrous sulfate solution, stirring for 5-15min, and performing suction filtration to obtain a filtrate.
Step S12, adding reduced iron powder into the filtrate, adjusting the pH value to 3.5-4.5 by adding ammonia water, heating to 80-100 ℃, stirring for 1.5-2.5h, cooling, standing, adding a flocculating agent, and filtering to remove impurities to obtain a purified ferrous sulfate solution;
wherein, after the precipitator sodium sulfide is added, impurity ions Mn can be effectively removed 2+ But impurity ion Al 3+ And Ti 4+ The reaction is not complete and the precipitation is incomplete, so that the impurity ion Al in the filtrate is required 3+ And Ti 4+ Further removing to obtain a purified ferrous sulfate solution, so that the synthesized ferric phosphate has better performance. Adding ammonia water to make impurity ion Al 3+ And Ti 4+ Converting into hydroxide precipitate, filtering to remove precipitate to remove impurity ion Al 3+ And Ti 4+ And obtaining a purified ferrous sulfate solution. Wherein, impurity ions Al can be effectively reduced by using ammonia water to remove impurities 3+ And Ti 4+ So that impurity ion Al is contained 3+ And Ti 4+ The content of (A) is reduced to below 0.01 percent so as to complete the supply of ferrous sulfate.
Specifically, heating the filtrate to 80-100 ℃ under the condition of stirring, adding 0.5-1.5g of reduced iron powder, adjusting the pH of the filtrate to 3.5-4.5 by adding ammonia water, and stirring for 1.5-2.5h;
standing and cooling after stirring, adding the polyaniline as a flocculating agent, standing for 20-40min, and filtering to remove impurities to obtain a purified ferrous sulfate solution.
Wherein, reduced iron powder is added for reducing the partially oxidized Fe in the filtrate 3+ So as to improve the purity of the ferrous sulfate solution, the addition of the flocculating agent can promote the formation of flocculation and precipitation, which is beneficial to removing impurities in the filtrate, and saves time so as to shorten the period of industrial production.
Step S13, mixing the purified ferrous sulfate solution with hydrogen peroxide and a pyrimidine byproduct phosphoric acid solution to obtain a first mixed solution;
at present, a large amount of phosphoric acid as a byproduct is generated in chlorination reaction in pyrimidine synthesis, the discharge of phosphoric acid causes great environmental pollution and resource waste, and meanwhile, phosphoric acid is treated as waste acid, so that the cost is extremely high, and the economic cost of enterprises can be increased. The battery-grade iron phosphate is synthesized by taking the pyrimidine byproduct phosphoric acid as a raw material, so that the pollution of the pyrimidine byproduct phosphoric acid to the environment can be reduced, the production cost of the battery-grade iron phosphate can be reduced, the comprehensive utilization and resource recovery of the byproduct are realized, and the method is green and environment-friendly.
The chlorination reaction in the pyrimidine synthesis is to react phosphorus oxychloride with methylthiopyrimidine to generate dichloropyrimidine and a by-product phosphoric acid, wherein in the ordinary chlorination reaction, excessive phosphorus oxychloride is usually added to complete the reaction of methylthiopyrimidine, so that the by-product phosphoric acid contains a small amount of phosphorus oxychloride, the temperature is controlled below 30 ℃ through hydrolysis reaction, and deionized water is slowly added dropwise to remove a small amount of residual phosphorus oxychloride to generate hydrogen chloride and phosphoric acid.
In addition, 80-100ml of a pyrimidine byproduct phosphoric acid solution with the concentration of 30% -40% is added into the first mixed solution to control the iron-phosphorus ratio of the synthesized iron phosphate and improve the purity of the synthesized iron phosphate.
In addition, 20-30ml of hydrogen peroxide is added into the first mixed solution, and under certain conditions, bivalent ferrous ions are completely oxidized into trivalent ferric ions.
Step S14, mixing sodium hydroxide and ammonia water to obtain a second mixed solution;
wherein, the second mixed liquid is prepared by mixing sodium hydroxide and ammonia water to combine with hydrogen ions in the reaction kettle to generate water, the PH value of the reaction is controlled, when the PH value of the reaction is smaller, the synthesis speed of the ferric phosphate crystal is too slow, the synthesis time of the ferric phosphate is increased, and when the PH value of the reaction is larger, the second mixed liquid is easy to form Fe (OH) with ferric ions 3 Precipitation will increase the crystal grains of the synthesized ferric phosphate and affect the conductivity of the lithium battery.
S15, adding a surfactant into deionized water for dissolving, adding into a reaction kettle, heating and stirring;
the surfactant is CTAB (cetyl trimethyl ammonium bromide), the agglomeration phenomenon can be reduced by adding the surfactant, the mass of the surfactant is 0.5-1.5g, and when the mass of the surfactant is less, the particle size of the synthesized iron phosphate particles is larger, so that the conductivity of the lithium battery is influenced.
Specifically, 0.5-1.5g of surfactant is added into 40-60ml of deionized water to be dissolved to prepare surfactant solution;
adding the surfactant solution into a reaction kettle, and heating to 80-100 ℃ under the condition of stirring.
S16, slowly pumping the first mixed solution and the second mixed solution into the reaction kettle through a first pump pipe and a second pump pipe respectively, heating to 80-100 ℃, stirring for 1.5-2.5h, and performing suction filtration to obtain iron phosphate precipitate;
the method comprises the steps of adding a first mixed solution and a second mixed solution into a reaction kettle through a first pump pipe and a second pump pipe respectively, controlling the feeding speed of the first mixed solution and the second mixed solution through the difference of the diameters of the first pump pipe and the second pump pipe, controlling the diameter of the first pump pipe to be 20-30mm and the diameter of the second pump pipe to be 10-20mm, reacting ferrous sulfate with hydrogen peroxide and phosphoric acid under the condition of heating and stirring to generate ferric phosphate, sulfuric acid and water, and controlling the reaction condition to synthesize the ferric phosphate with small crystal grains and high purity, namely the ferric phosphate with the iron-phosphorus molar ratio meeting the requirement.
In addition, the pH value of the reaction environment in the reaction kettle is adjusted to be 1.5-2.3 by the second mixed liquid, when the pH value of the reaction is small, the synthesis speed of the iron phosphate crystal is too slow, the synthesis time of the iron phosphate is prolonged, and when the pH value of the reaction is large, fe (OH) is easily formed by the second mixed liquid and ferric ions 3 Precipitation will increase the crystal grains of the synthesized ferric phosphate and affect the conductivity of the lithium battery.
And S17, washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times to obtain the battery-grade iron phosphate.
The pyrimidine by-product phosphoric acid contains impurity ions, namely chloride ions and sulfate ions in ferrous sulfate, and the impurity ions are brought into iron phosphate precipitation, so that the iron phosphate needs to be subjected to impurity removal to obtain battery-grade iron phosphate.
Specifically, the method comprises the step of calculating through a solubility product formula by utilizing different solubility products of different ions in an ammonia water solution to obtain that impurity ions in the iron phosphate precipitate can be preferentially dissolved in the ammonia water solution with preset concentration.
Firstly, by looking up the solubility of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate at 25 ℃, obtaining a concentration value C of a saturated solution of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate according to the following saturated solution concentration calculation formula;
wherein S is the solubility of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate in water, M is the molar mass of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate, and rho is the density of saturated solution of ammonium phosphosulfate, ammonium chloride and ammonium dihydrogen phosphate.
Then, the solubility product K of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate is obtained according to the following solubility product calculation formula sp ；
K SP ＝C 1 ×C 2
Wherein, C 1 Is the concentration of ammonium ions in saturated solution of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate, C 2 The concentrations of sulfate ions, chloride ions and dihydrogen phosphate ions in saturated solution of ammonium sulfate, ammonium chloride and ammonium dihydrogen phosphate are shown.
Finally, obtaining the dissolved concentrations C of different ions of the ammonia water solution under the preset concentration according to the following concentration calculation formula 2 * ；
Wherein, C 1 * The molar concentration of ammonium ions in the ammonia water solution with the preset concentration.
It is calculated that in the ammonia water solution with the preset concentration of 0.05-0.15%, the molar concentrations of the sulfate ions, the chloride ions and the dihydrogen phosphate ions are larger than that of the chloride ions, and therefore, the sulfate ions and the chloride ions can be preferentially dissolved in the ammonia water solution with the preset concentration of 0.05-0.15% by deduction.
And washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times, and preferentially removing impurity ions to obtain the battery-grade iron phosphate. The battery-grade iron phosphate is obtained by washing, filtering and drying for 5-15 times in an ammonia water solution with the preset concentration of 0.05% -0.15% to remove impurity ions, so that the content of sulfate ions and chloride ions is lower than 0.01%. The method is simple, environment-friendly and easy for large-scale production, and when the preset concentration is too high, the phosphate ions can be dissolved after the sulfate ions and the chloride ions of the impurity ions are completely dissolved, so that the yield of the battery-grade iron phosphate is reduced, the cost is increased, and the industrial mass production is not facilitated. When the preset concentration is too low, the number of times of washing is increased, time is consumed, and cost is increased. When the washing times are excessive, the phosphate ions are dissolved after the sulfate ions and the chloride ions of the impurity ions are completely dissolved, so that the yield of the battery-grade iron phosphate is reduced, the cost is increased, and the industrial mass production is not facilitated; when the washing times are too few, impurity ions cannot be completely removed, so that the purity of the iron phosphate is not high, and various performances of the iron phosphate are influenced.
In this embodiment, the predetermined number of times is 10, and the predetermined concentration is 0.1%.
Compared with the prior art, the method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid has the advantages that: according to the method for synthesizing the battery-grade iron phosphate by using the byproduct ferrous sulfate and the byproduct phosphoric acid, the battery-grade iron phosphate is prepared by using the byproduct ferrous sulfate of titanium white and the byproduct phosphoric acid of pyrimidine as raw materials, so that the recycling of the byproduct ferrous sulfate of titanium white and the byproduct phosphoric acid of pyrimidine is realized, the iron phosphate with high purity and small crystal grains is prepared, the requirements of the battery-grade iron phosphate are met, and the method is economical and environment-friendly.
Example two
A second embodiment of the present invention provides a method for synthesizing battery-grade iron phosphate from a byproduct of ferrous sulfate and a byproduct of phosphoric acid, which is different from the method for synthesizing battery-grade iron phosphate from a product of ferrous sulfate and a byproduct of phosphoric acid in the first embodiment in that:
the preset concentration is 0.5%.
EXAMPLE III
A third embodiment of the present invention provides a method for synthesizing battery-grade iron phosphate from a byproduct of ferrous sulfate and a byproduct of phosphoric acid, which is different from the method for synthesizing battery-grade iron phosphate from a product of ferrous sulfate and a byproduct of phosphoric acid in the first embodiment in that:
the preset concentration is 0.15%.
Example four
A fourth embodiment of the present invention provides a method for synthesizing battery-grade iron phosphate from a byproduct of ferrous sulfate and a byproduct of phosphoric acid, which is different from the method for synthesizing battery-grade iron phosphate from a product of ferrous sulfate and a byproduct of phosphoric acid in the first embodiment in that:
the preset number of times is 5.
EXAMPLE five
A fifth embodiment of the present invention provides a method for synthesizing battery-grade iron phosphate from a byproduct of ferrous sulfate and a byproduct of phosphoric acid, where the method is different from the method for synthesizing battery-grade iron phosphate from a product of ferrous sulfate and a byproduct of phosphoric acid in the first embodiment in that:
the preset number of times is 15.
Please refer to table 1 below, which shows the parameters corresponding to the first to fifth embodiments of the present invention.
Table 1:
| item | Preset concentration | Predetermined number of times | Concentration of sulfate ion | Concentration of chloride ion |
| Example one | 0.1％ | 10 | ≦0.01％ | ≦0.01％ |
| Example two | 0.05％ | 10 | 0.020％ | 0.034％ |
| EXAMPLE III | 0.15％ | 10 | ≦0.01％ | ≦0.01％ |
| Example four | 0.1％ | 5 | ≦0.01％ | 0.026％ |
| EXAMPLE five | 0.1％ | 15 | ≦0.01％ | ≦0.01％ |
As can be seen from the data of the first to third embodiments, under the condition that the preset number of times is 10, the preset concentration is too low, the ammonia solution cannot completely dissolve the sulfate ions and the chloride ions, and the concentration of the impurity ions cannot be reduced to less than 0.01%, so that the purity of the iron phosphate is not high, and the iron phosphate does not meet the requirement of battery-grade iron phosphate, thereby affecting the performance of the iron phosphate applied to the battery. When the preset concentration is too high, the impurity ions, namely sulfate ions and chloride ions, can be completely dissolved, so that the concentration of the impurity ions is reduced to be less than 0.01 percent, the concentration of the phosphate ions can be reduced, the yield of the battery-grade iron phosphate is reduced, the cost is increased, and the industrial mass production is not facilitated.
By combining the data of the first embodiment, the fourth embodiment and the fifth embodiment, it is known that, under the condition that the preset concentration is 0.1%, the preset times are too low, the ammonia water solution cannot completely dissolve sulfate ions and chloride ions, and the concentration of the impurity ions cannot be reduced to less than 0.01%, so that the purity of the iron phosphate is not high, and the requirement of battery-grade iron phosphate is not met, thereby affecting the performance of the iron phosphate applied to the battery. When the preset times are too high, impurity ions are removed, but the performance improvement effect on the battery-grade iron phosphate is not obvious, but the process flow is increased, the process time is increased, and the process cost is increased.
In conclusion, the iron phosphate precipitate is synthesized by adopting the ferrous sulfate as the titanium white byproduct and the phosphoric acid as the pyrimidine byproduct, and impurities in the iron phosphate precipitate are removed according to different solubility products with an ammonia water solution, so as to synthesize the iron phosphate meeting the requirement of the iron-phosphorus ratio, namely the iron phosphate with high purity and small particle size, and the titanium white byproduct and the pyrimidine byproduct are recycled, so that the cost is low, the production cost of the lithium ion battery is reduced, the synthesis method is simple, green and environment-friendly, the industrial large-scale production is facilitated, the pollution and the resource waste of the titanium white byproduct and the pyrimidine byproduct are avoided, and the production cost of the iron source and the phosphoric acid source is reduced.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for synthesizing battery grade iron phosphate from a byproduct ferrous sulfate and a byproduct phosphoric acid, the method comprising:
adding deionized water into titanium dioxide byproduct ferrous sulfate for dissolving, and filtering to remove insoluble impurities to obtain a ferrous sulfate solution;
adding a sodium sulfide solution into the ferrous sulfate solution, stirring and filtering to obtain a filtrate;
adding reduced iron powder into the filtrate, adjusting the pH value to 3.5-4.5 by adding ammonia water, heating to 80-100 ℃, stirring for 1.5-2.5h, cooling, standing, adding a flocculating agent, and filtering to remove impurities to obtain a purified ferrous sulfate solution;
mixing the purified ferrous sulfate solution with hydrogen peroxide and a pyrimidine by-product phosphoric acid solution to obtain a first mixed solution;
mixing sodium hydroxide and ammonia water to obtain a second mixed solution;
adding a surfactant into deionized water for dissolving, adding into a reaction kettle, heating and stirring;
slowly pumping the first mixed solution and the second mixed solution into the reaction kettle through a first pump pipe and a second pump pipe respectively, heating to 80-100 ℃, stirring for 1.5-2.5h, and performing suction filtration to obtain iron phosphate precipitate;
and washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times to obtain the battery-grade iron phosphate.
2. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the step of washing, filtering and drying the iron phosphate precipitate with an ammonia water solution with a preset concentration for a preset number of times to obtain the battery-grade iron phosphate comprises the following steps:
calculating by using different solubility products of different ions in the ammonia water solution according to a solubility product formula to obtain that impurity ions in the iron phosphate precipitate can be preferentially dissolved in the ammonia water solution with preset concentration;
and washing, filtering and drying the iron phosphate precipitate by using an ammonia water solution with preset concentration for preset times, and preferentially removing impurity ions to obtain the battery-grade iron phosphate.
3. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 2, wherein the preset concentration of the ammonia water solution is 0.05% -0.15%, and the preset times are 5-15%.
4. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the step of dissolving the byproduct ferrous sulfate of titanium dioxide in deionized water, and filtering to remove insoluble impurities to obtain a ferrous sulfate solution specifically comprises:
adding 75-95g of ferrous sulfate serving as a titanium white byproduct into 300-500ml of deionized water, and stirring for dissolving;
insoluble impurities in the solution were removed by filtration to obtain a ferrous sulfate solution.
5. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the step of adding sodium sulfide to the ferrous sulfate solution, stirring and filtering to obtain a filtrate specifically comprises:
dissolving sodium sulfide in deionized water to prepare 40-60ml of sodium sulfide solution with the concentration of 20-40 g/L;
and adding the sodium sulfide solution into the ferrous sulfate solution, stirring for 5-15min, and carrying out suction filtration to obtain a filtrate.
6. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the steps of adding reduced iron powder into the filtrate, adjusting the pH to 3.5-4.5 by adding ammonia water, heating to 80-100 ℃, stirring for 1.5-2.5h, cooling, standing, adding a flocculating agent, and filtering to remove impurities to obtain a purified ferrous sulfate solution specifically comprise:
heating the filtrate to 80-100 ℃ under the condition of stirring, adding 0.5-1.5g of reduced iron powder, adjusting the pH of the filtrate to 3.5-4.5 by adding ammonia water, and stirring for 1.5-2.5h;
standing and cooling after stirring, adding the polyaniline as flocculant, standing for 20-40min, and filtering to remove impurities to obtain a purified ferrous sulfate solution.
7. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the addition amount of the hydrogen peroxide is 20-30ml, the concentration of the pyrimidine byproduct phosphoric acid solution is 30% -40%, and the addition amount is 80-100ml.
8. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the step of adding a surfactant into deionized water for dissolving, and adding the dissolved surfactant into a reaction kettle for heating and stirring comprises the following steps:
adding surfactant with the mass of 0.5-1.5g into deionized water of 40-60ml for dissolving to prepare surfactant solution;
adding the surfactant solution into a reaction kettle, and heating to 80-100 ℃ under the condition of stirring.
9. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the diameter of the first pump tube is 20-30mm, and the diameter of the second pump tube is 10-20mm.
10. The method for synthesizing battery-grade iron phosphate from the byproduct ferrous sulfate and the byproduct phosphoric acid according to claim 1, wherein the second mixed solution is pumped into the reaction kettle to control the pH of the reaction environment to be between 1.5 and 2.3.
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