CN115707650A - Production process of iron phosphate with phosphorus-containing polymeric ferric sulfate as precursor - Google Patents
Production process of iron phosphate with phosphorus-containing polymeric ferric sulfate as precursor Download PDFInfo
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- CN115707650A CN115707650A CN202110946043.9A CN202110946043A CN115707650A CN 115707650 A CN115707650 A CN 115707650A CN 202110946043 A CN202110946043 A CN 202110946043A CN 115707650 A CN115707650 A CN 115707650A
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- phosphate
- phosphorus
- ferric sulfate
- polymeric ferric
- iron
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 title claims abstract description 55
- 229910000360 iron(III) sulfate Inorganic materials 0.000 title claims abstract description 55
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 52
- 239000011574 phosphorus Substances 0.000 title claims abstract description 52
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims abstract description 45
- 239000002243 precursor Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 229910000398 iron phosphate Inorganic materials 0.000 title claims description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000005955 Ferric phosphate Substances 0.000 claims abstract description 15
- 229940032958 ferric phosphate Drugs 0.000 claims abstract description 15
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 9
- 239000010452 phosphate Substances 0.000 claims abstract description 9
- 150000001450 anions Chemical class 0.000 claims abstract description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- 229910052742 iron Inorganic materials 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 4
- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 claims description 4
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 3
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 3
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 239000004254 Ammonium phosphate Substances 0.000 claims description 2
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 2
- 239000003818 cinder Substances 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- 235000019797 dipotassium phosphate Nutrition 0.000 claims description 2
- 229910000396 dipotassium phosphate Inorganic materials 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000014413 iron hydroxide Nutrition 0.000 claims description 2
- 235000013980 iron oxide Nutrition 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 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
- 235000011007 phosphoric acid 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
- 229910000160 potassium phosphate Inorganic materials 0.000 claims description 2
- 235000011009 potassium phosphates Nutrition 0.000 claims description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052683 pyrite Inorganic materials 0.000 claims description 2
- 239000011028 pyrite Substances 0.000 claims description 2
- 239000002994 raw material Substances 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
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 235000011008 sodium phosphates Nutrition 0.000 claims description 2
- 239000007787 solid Substances 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
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 abstract description 5
- 239000011593 sulfur Substances 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 238000005406 washing Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 2
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- LFHUEDOICHSCGP-UHFFFAOYSA-L [O-]P([O-])(O)=O.S.[Fe+2] Chemical compound [O-]P([O-])(O)=O.S.[Fe+2] LFHUEDOICHSCGP-UHFFFAOYSA-L 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- 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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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a production process of ferric phosphate by taking phosphorus-containing polymeric ferric sulfate as a precursor. The molecular formula of the polymeric ferric sulfate containing phosphorus can be expressed as Fe (OH) n SO 4 (PO 4 ) (1‑n)/3 Besides traditional hydroxide radical and sulfate radical, phosphate radical is also introduced into the anion. When the phosphorus-containing polymeric ferric sulfate is used as a precursor to produce the ferric phosphate, the production cost and the sulfur content of the coated ferric phosphate can be effectively reduced. The ferric phosphate produced by the method can be used as an excellent precursor of lithium iron phosphate as a positive material of a lithium ion battery.
Description
The technical field is as follows:
the invention relates to a production process of ferric phosphate by taking phosphorus-containing polymeric ferric sulfate as a precursor.
Background art:
china needs to realize carbon peak reaching in 2030 years and realize carbon neutralization in 2060 years. Therefore, new energy markets represented by wind power, photoelectricity, lithium ion batteries and the like are rapidly developed in the year. Lithium ion batteries based on lithium iron phosphate have developed rapidly due to their excellent safety performance, and the sales of lithium iron phosphate up to the end of 6 months in 2021 have exceeded the sum of sales throughout the year, and the market is still in a state of short supply and short demand. As the most important precursor of lithium iron phosphate, the production of iron phosphate is limited by the capacity expansion cycle, and is also in a short supply and demand state. However, in the foreseeable future, the market competition of iron phosphate will be intensified as the new production capacity of each production enterprise is gradually released. How to produce high-quality iron phosphate at lower cost plays a crucial role in improving product competitiveness and stabilizing market share.
Polymeric ferric sulfate is a common precursor for the synthesis of ferric phosphate. For example, chinese patent CN 102120569A reports a synthetic process of iron phosphate which uses polymeric ferric sulfate as iron source, has low cost and can be industrially and continuously produced. In the process, polymeric ferric sulfate and phosphoric acid are mixed and stirred, and a finished product of ferric phosphate can be obtained by controlling the pH value and the reaction time of the solution, filtering, washing and drying; chinese patent CN 111362242A reports a process method for preparing iron phosphate with large specific surface area by using polymeric ferric sulfate, and the specific surface area of the prepared iron phosphate reaches 20m 2 More than g. Chinese patent CN 102050435A reports a process for preparing iron phosphate by using polymeric ferric sulfate, the purity of the prepared iron phosphate is more than 99%, the particle size is fine and uniform, and the process is particularly suitable for producing lithium iron phosphate as a lithium ion anode material. However, patents have all reported the use of sulfuric acid as a basicity modifier for ferric polysulfate, whose molecular formula may be abbreviated as Fe 2 (OH) n SO 4(6-n)/2 In which SO 4 2- With Fe 3+ Is greater than 1. Considering that the subsequent synthesis of iron phosphate by using polymeric ferric sulfate still needs to be mixed with phosphorus salt, in the preparation stage of polymeric ferric sulfate, namely, phosphoric acid is used as a salt basicity regulator of the polymeric ferric sulfate instead of sulfuric acid, so that the production cost of the iron phosphate can be obviously reduced.
The invention content is as follows:
the invention aims to provide a production process of iron phosphate by using phosphorus-containing polymeric ferric sulfate as a precursor so as to further reduce the production cost of the iron phosphate and the content of sulfate radicals coated in a product.
The technical scheme of the invention is as follows.
A production process of ferric phosphate by using phosphorus-containing polymeric ferric sulfate as a precursor. The method is characterized in that phosphorus-containing polymeric ferric sulfate is used as an iron source, phosphate is used as a phosphorus source, and battery-grade ferric phosphate is produced by controlling the reaction temperature and the pH value;
the anion of the phosphorus-containing polymeric ferric sulfate contains phosphate radical, hydrogen phosphate radical or dihydrogen phosphate radical;
the raw material of the phosphorus-containing polymeric ferric sulfate can be one or more of ferrous sulfate, iron oxide, iron hydroxide and pyrite cinder;
the iron content of the phosphorus-containing polymeric ferric sulfate is 1-20%;
the molar ratio of phosphate radicals to sulfate radicals in the polymeric ferric sulfate containing phosphorus is 0.01-5;
the pH value of the phosphorus-containing polymeric ferric sulfate is-1.0-2.0;
the phosphorus-containing polymeric ferric sulfate can be in a liquid state or a solid state;
the phosphate can be one or more of phosphoric acid, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate and potassium phosphate;
the reaction temperature is 25-95 ℃;
the reaction pH is 0.5-3.5;
the reaction time is 0.5 to 10 hours.
The invention has the beneficial effects that: phosphoric acid is used for replacing sulfuric acid when the phosphorus-containing polymeric ferric sulfate is prepared, so that the use of sulfuric acid is avoided, and the cost is reduced; when the phosphorus-containing polymeric ferric sulfate is used as an iron source to prepare the ferric phosphate, the alkali consumption is reduced, and the cost is further reduced; because sulfuric acid is not introduced during the preparation of the phosphorus-containing polymeric ferric sulfate, when the phosphorus-containing polymeric ferric sulfate is used for preparing the ferric phosphate, the sulfate radical content in a reaction system is lower than that of the reaction system based on the traditional polymeric ferric sulfate, the reduction of the washing water amount is facilitated, and the prepared ferric phosphate has lower sulfur content.
Description of the drawings:
FIG. 1 SEM photograph of iron phosphate prepared in example 1;
figure 2 XRD pattern of iron phosphate made in example 1.
The specific implementation mode is as follows:
the examples should not be construed as limiting the scope of the invention.
Example 1
500g (1.8 mol) of ferrous sulfate heptahydrate is dissolved in 500g of pure water, 58g (0.5 mol) of 85% phosphoric acid and 32g (0.3 mol) of sodium chlorate are added under stirring, and after high-temperature curing, the phosphorus-containing polymeric ferric sulfate is prepared, wherein the iron content is 9.2%. Taking the phosphorus-containing polymeric ferric sulfate as an iron source, taking 150g (1.3 mol) of phosphoric acid as a phosphorus source, mixing, adding pure water to dilute to 2L, adjusting the pH value of the solution to 1.5 by using liquid alkali, controlling the reaction temperature to be 85 ℃, filtering after reacting for 6 hours, washing a filter cake until the conductivity is less than or equal to 200 mu S, and drying at 105 ℃ to constant weight.
As shown in fig. 1 and 2, SEM and XRD patterns of the iron phosphate obtained in this example show that the obtained iron phosphate secondary particles are spheroidal, the primary particles are fine ellipsoids, and the adhesion between the particles is very small, and the particle size of the primary particles is between 50 nm and 100 nm. As can be seen from XRD, the iron phosphate synthesized in this example is high-crystallinity ferric phosphate dihydrate (FePO) 4 .2H 2 O), the map is matched with a standard card #033-0666, and the strain belongs to a monoclinic system.
Example 2
500g (1.8 mol) of ferrous sulfate heptahydrate is dissolved in 1000g of pure water, 23g (0.2 mol) of 85% phosphoric acid and 113g (1 mol) of 30% hydrogen peroxide are added under stirring, and the phosphorus-containing polymeric ferric sulfate is prepared after high-temperature curing, wherein the iron content is 6.1%. Taking the phosphorus-containing polymeric ferric sulfate as an iron source, taking 184.5g (1.6 mol) of phosphoric acid as a phosphorus source, mixing, adding pure water to dilute to 2L, adjusting the pH value of the solution to 1.8 by using liquid caustic soda, controlling the reaction temperature to be 70 ℃, filtering after reacting for 10 hours, washing a filter cake until the conductivity is less than or equal to 200 mu S, and drying at 105 ℃ to constant weight.
Example 3
200g of pure water is added into 500g (1.8 mol) of ferrous sulfate heptahydrate, 115g (1 mol) of 85% phosphoric acid and 113g (1 mol) of 30% hydrogen peroxide are added under stirring, and the phosphorus-containing polymeric ferric sulfate is prepared after high-temperature curing, wherein the iron content is 10.8%. Taking the phosphorus-containing polymeric ferric sulfate as an iron source, taking 92g (0.8 mol) of ammonium dihydrogen phosphate as a phosphorus source, mixing, adding pure water to dilute to 2L, adjusting the pH value of the solution to 2.0 by using ammonia water, controlling the reaction temperature to be 90 ℃, filtering after reacting for 5 hours, washing a filter cake until the conductivity is less than or equal to 200 mu S, and drying at 105 ℃ to constant weight.
Comparative example
500g (1.8 mol) of ferrous sulfate heptahydrate is dissolved in 500g of pure water, 60g (0.6 mol) of 98% concentrated sulfuric acid and 32g (0.3 mol) of sodium chlorate are added under stirring, and the mixture is cured at high temperature to prepare polymeric ferric sulfate, wherein the iron content is 9.2%. Taking the polymeric ferric sulfate as an iron source, taking 150g (1.8 mol) of phosphoric acid as a phosphorus source, mixing, adding pure water to dilute to 2L, adjusting the pH value of the solution to 1.5 by using liquid alkali, controlling the reaction temperature to be 85 ℃, filtering after reacting for 6 hours, washing a filter cake until the conductivity is less than or equal to 200 mu S, and drying at 105 ℃ to constant weight.
The iron content, phosphorus content, iron-phosphorus ratio and sulfur content of example 1, example 2, example 3 and comparative example were measured, respectively, and the results are shown in the following table. Wherein, the iron content test adopts a potassium dichromate titration method, the phosphorus content test adopts a quinomolybdyl-citranone precipitation method, and the sulfur content test adopts a high-frequency infrared combustion method.
From the data, the iron content, the phosphorus content and the iron-phosphorus ratio of the examples of the invention are slightly different from those of the comparative examples, but the sulfur content of the iron phosphate product can be controlled to be within 100ppm by the examples 1 to 3 of the invention. Compared with the prior art, the content of the iron phosphate sulfur prepared by adopting the traditional polymeric ferric sulfate almost reaches 2 times of that of the embodiment.
Claims (11)
1. A production process of ferric phosphate with phosphorus-containing polymeric ferric sulfate as a precursor is characterized in that the phosphorus-containing polymeric ferric sulfate is used as an iron source, phosphate is used as a phosphorus source, and battery-grade ferric phosphate is produced by controlling the reaction temperature and the pH value.
2. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the anion of the phosphorus-containing polymeric ferric sulfate contains phosphate radical, hydrogen phosphate radical or dihydrogen phosphate radical.
3. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the raw material of the phosphorus-containing polymeric ferric sulfate can be one or more of ferrous sulfate, iron oxide, iron hydroxide and pyrite cinder.
4. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the iron content of the phosphorus-containing polymeric ferric sulfate is 1% -20%.
5. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the molar ratio of phosphate radicals to sulfate radicals in the phosphorus-containing polymeric ferric sulfate is 0.01 to 5.
6. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the pH value of the phosphorus-containing polymeric ferric sulfate is minus 1.0 to 2.0.
7. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the polymeric ferric sulfate containing phosphorus can be in a liquid state or a solid state.
8. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the phosphate can be one or more of phosphoric acid, ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, ammonium phosphate, sodium monohydrogen phosphate, sodium dihydrogen phosphate, sodium phosphate, potassium monohydrogen phosphate, potassium dihydrogen phosphate and potassium phosphate.
9. The production process of iron phosphate using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, characterized in that: the reaction temperature is 25-95% o C。
10. The production process of iron phosphate using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, characterized in that: the reaction pH is 0.5 to 3.5.
11. The process for producing iron phosphate by using polymeric ferric sulfate containing phosphorus as a precursor according to claim 1, wherein the process comprises the following steps: the reaction time is 0.5 to 10 hours.
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|---|---|---|---|---|
| JP2000191328A (en) * | 1998-12-25 | 2000-07-11 | Taki Chem Co Ltd | Production of ferric sulfate solution |
| CN101531355A (en) * | 2009-04-22 | 2009-09-16 | 广西大学 | Method for preparing high purity ferric phosphate using ferrous sulfate as by-product of white titanium pigment |
| CN101805051A (en) * | 2010-04-06 | 2010-08-18 | 重庆大学 | Compound phosphoric polyferric sulfate flocculant and production method thereof |
| CN102050435A (en) * | 2010-12-13 | 2011-05-11 | 易玲 | Production method of battery-grade iron phosphate |
| CN102120569A (en) * | 2011-01-31 | 2011-07-13 | 李宝峰 | Preparation method of ferric phosphate |
| JP2013127898A (en) * | 2011-12-19 | 2013-06-27 | Taiheiyo Cement Corp | Method for producing lithium ion secondary battery anode active material |
| CN112960662A (en) * | 2021-03-04 | 2021-06-15 | 深圳市长隆科技有限公司 | Green and environment-friendly production process of iron phosphate |
-
2021
- 2021-08-18 CN CN202110946043.9A patent/CN115707650A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000191328A (en) * | 1998-12-25 | 2000-07-11 | Taki Chem Co Ltd | Production of ferric sulfate solution |
| CN101531355A (en) * | 2009-04-22 | 2009-09-16 | 广西大学 | Method for preparing high purity ferric phosphate using ferrous sulfate as by-product of white titanium pigment |
| CN101805051A (en) * | 2010-04-06 | 2010-08-18 | 重庆大学 | Compound phosphoric polyferric sulfate flocculant and production method thereof |
| CN102050435A (en) * | 2010-12-13 | 2011-05-11 | 易玲 | Production method of battery-grade iron phosphate |
| CN102120569A (en) * | 2011-01-31 | 2011-07-13 | 李宝峰 | Preparation method of ferric phosphate |
| JP2013127898A (en) * | 2011-12-19 | 2013-06-27 | Taiheiyo Cement Corp | Method for producing lithium ion secondary battery anode active material |
| CN112960662A (en) * | 2021-03-04 | 2021-06-15 | 深圳市长隆科技有限公司 | Green and environment-friendly production process of iron phosphate |
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