CN115535988B - Preparation method of flaky cobalt phosphate - Google Patents
Preparation method of flaky cobalt phosphate Download PDFInfo
- Publication number
- CN115535988B CN115535988B CN202211466835.7A CN202211466835A CN115535988B CN 115535988 B CN115535988 B CN 115535988B CN 202211466835 A CN202211466835 A CN 202211466835A CN 115535988 B CN115535988 B CN 115535988B
- Authority
- CN
- China
- Prior art keywords
- cobalt
- phosphoric acid
- solution
- cobalt phosphate
- flaky
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910000152 cobalt phosphate Inorganic materials 0.000 title claims abstract description 43
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000243 solution Substances 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 32
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 150000001868 cobalt Chemical class 0.000 claims abstract description 15
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 13
- 229940044175 cobalt sulfate Drugs 0.000 claims description 10
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 10
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 239000012459 cleaning agent Substances 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 239000002243 precursor Substances 0.000 abstract description 14
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QOQSIXJUYVUEMP-UHFFFAOYSA-H cobalt(2+);diphosphate;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QOQSIXJUYVUEMP-UHFFFAOYSA-H 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002562 thickening agent Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- ASYZRLCMYUFCHK-UHFFFAOYSA-N azane cobalt phosphoric acid Chemical compound N.[Co].OP(O)(O)=O ASYZRLCMYUFCHK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- GIPIUENNGCQCIT-UHFFFAOYSA-K cobalt(3+) phosphate Chemical group [Co+3].[O-]P([O-])([O-])=O GIPIUENNGCQCIT-UHFFFAOYSA-K 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of flaky cobalt phosphate, which takes a phosphoric acid aqueous solution with a certain concentration as a base solution, and flows a soluble cobalt salt solution, a phosphoric acid aqueous solution and ammonia water into a reaction kettle, and strictly controls the pH value of a reaction system in two stages to react, so that the preparation of flaky cobalt phosphate precursor with high purity, uniform particle size distribution and thin thickness is realized. The method has the advantages of good process controllability, good reproducibility, low energy consumption and high mass production degree.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of flaky cobalt phosphate.
Background
In recent years, cobalt phosphate has been receiving attention due to its wide application in the fields of catalysis, lithium ion batteries, supercapacitors and the like, and has become a promising phosphate.
Currently, the method for synthesizing cobalt phosphate is mainly a hydrothermal method. Cobalt phosphate microspheres were synthesized using a hydrothermal process as in patent 201810140016.0. In the 201810832501.4 patent, a hydrothermal method is adopted to synthesize the nano material with the thickness of 0.5-1 mu m. And a surfactant is usually added in the hydrothermal synthesis process to regulate the morphology and the size of the material, and the synthesis yield is low, the energy consumption is high and the cost is high.
Although the cobalt phosphate is synthesized by a wet precipitation process without adding a surfactant or a thickener in the patent 201410453227.1, the synthesized cobalt phosphate has larger size, the median particle diameter is 3-13 um, and the morphology is irregular blocky or thick-plate-shaped intercalation flower-shaped, and the morphology uniformity is poor.
In a word, the existing preparation method of the flaky cobalt phosphate has the technical problems of low yield, high energy consumption and cost, or irregular or thick prepared material morphology and the like.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a preparation method of flaky cobalt phosphate.
A preparation method of flaky cobalt phosphate comprises the following steps:
s1, preparing a cobalt salt solution and a phosphoric acid aqueous solution for later use;
s2, taking a phosphoric acid aqueous solution with a certain concentration as a base solution, flowing the soluble cobalt salt solution, the phosphoric acid aqueous solution and ammonia water prepared in the step S1 into a reaction kettle, reacting, controlling the pH value of a reaction system to be 4.0-6.0, continuing stirring for a reaction time period t1 after the feeding of the soluble cobalt salt solution and the phosphoric acid aqueous solution is finished, adjusting the inflow of the ammonia water to adjust the pH value of the reaction system to be 7.0-9.0, and stirring for a reaction time period t2;
and S3, washing and drying the obtained material, and then calcining at high temperature to obtain the flaky cobalt phosphate.
Preferably, in the step S2, the adding amount of the base solution accounts for 10-50% of the total volume of the reaction kettle, and the pH value of the base solution is 4.0-6.0.
Preferably, in the step S2, the feeding amount of the cobalt salt solution is 250-500 mL/min; the feeding amount of the phosphoric acid solution is 16.7-153.3 mL/min.
Preferably, in the step S2, the reaction temperature is 30-50 ℃ and the stirring linear velocity is 5-11 m/S.
Preferably, in the step S2, the feeding time of the cobalt salt solution and the phosphoric acid aqueous solution is 0.5-1 h; t1 is 10-30 min; and t2 is 0.5-2 h.
Preferably, the mass percentage of ammonia in the ammonia water is 25-28%.
Preferably, in step S3, the high-temperature calcination is: the temperature is kept for 0.5 to 1 hour at 200 to 300 ℃ and then is kept for 1 to 4 hours at 550 to 650 ℃. When the calcination temperature of high-temperature calcination is lower than 550 ℃, the crystal water in the wet-process synthesized precursor cannot be completely removed, and when the temperature is higher than 650 ℃, the wet-process synthesized precursor is obviously sintered.
Optionally, the cobalt salt is one or more of cobalt sulfate, cobalt chloride, cobalt nitrate and cobalt acetate.
Preferably, the concentration of the cobalt salt solution is 1.0-2.0 mol/L; the concentration of the phosphoric acid solution is 5-10 mol/L.
Preferably, in step S3, pure water is used as a cleaning agent for the washing; the consumption of the washing water is controlled to be 1:5-10 kg/L of total solid-liquid ratio; the drying is vacuum drying.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, under the condition that no surfactant or thickener is introduced, a wet precipitation process is adopted to synthesize the flaky cobalt phosphate material, and the reaction pH at different stages is strictly controlled by adopting a phosphoric acid aqueous solution with a certain concentration as a base solution, so that the preparation of the flaky cobalt phosphate precursor with high purity, uniform particle size distribution and thin thickness is realized. The method has the advantages of good process controllability, good reproducibility, low energy consumption and high mass production degree.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of a cobalt phosphate precursor after completion of the wet reaction of example 1;
FIG. 2 is an SEM image of calcined cobalt phosphate prepared according to example 1;
FIG. 3 is an XRD pattern of cobalt phosphate before and after calcination prepared in example 1;
FIG. 4 is an SEM image of a cobalt phosphate precursor after completion of the wet reaction of example 2;
FIG. 5 is an SEM image of a cobalt phosphate precursor after completion of the wet reaction of comparative example 1;
FIG. 6 is an SEM image of calcined cobalt phosphate of comparative example 1;
FIG. 7 is an XRD pattern of cobalt phosphate before and after calcination prepared in comparative example 1;
fig. 8 is an SEM image of the cobalt phosphate precursor after the wet reaction of comparative example 2 is completed.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings and preferred embodiments in order to facilitate an understanding of the invention, but the scope of the invention is not limited to the following specific embodiments.
Example 1:
step S1: preparing a cobalt sulfate solution with the concentration of 1mol/L and a phosphoric acid solution with the concentration of 10mol/L for later use;
step S2: taking aqueous solution with pH of 6.0 adjusted by phosphoric acid as base solution, wherein the addition amount of the base solution is 50% of the total volume of the reaction kettle, controlling the reaction temperature of the system to be 30 ℃, and controlling the stirring linear speed to be 5m/s. And (3) adding the cobalt sulfate solution, the phosphoric acid solution and ammonia water (the mass percent of ammonia is 25-28%) into a reaction kettle in parallel, wherein the feeding amount of the cobalt sulfate solution is 250mL/min, the feeding amount of the phosphoric acid solution is 16.7mL/min, the pH of the reaction process is controlled to be 6.0 by the ammonia water, and the total feeding time is 1h. Stirring is continued for 10min after the end of feeding. The reaction temperature of the system is controlled to be 30 ℃, the reaction pH of the ammonia water is adjusted to be 9.0, and the stirring is continued for 0.5h;
step S3: centrifugally washing the material in the step S2 by pure water, controlling the total solid-to-liquid ratio to be 1:10kg/L, centrifugally dehydrating, and vacuum drying at 110 ℃;
step S6: and (3) preserving heat of the material in the step (S3) for 1h at 200 ℃ and preserving heat for 4h at 550 ℃ to obtain the anhydrous cobalt phosphate.
From fig. 1 and 2, the cobalt phosphate has a lamellar morphology, the particle size distribution is uniform as a whole, and no obvious ultra-large lamellar morphology exists. XRD of fig. 3 shows that the precursor before calcination is cobalt phosphate octahydrate and the precursor after calcination is cobalt phosphate anhydrous structure.
Example 2:
step S1: preparing a cobalt chloride solution with the concentration of 2mol/L and a phosphoric acid solution with the concentration of 5 mol/L for later use;
step S2: taking aqueous solution with pH of 4.0 adjusted by phosphoric acid as base solution, wherein the addition amount of the base solution is 50% of the total volume of the reaction kettle, controlling the reaction temperature of the system to be 50 ℃, and controlling the stirring linear speed to be 11m/s. And (3) co-current adding a cobalt chloride solution, a phosphoric acid solution and ammonia water (the mass percentage of ammonia is 25-28%) into a reaction kettle, wherein the feeding amount of the cobalt chloride solution is 500mL/min, the feeding amount of the phosphoric acid solution is 153.3mL/min, the pH of the reaction process is controlled to be 4.0 by the ammonia water, and the total feeding time is 0.5h. Stirring is continued for 30min after the feeding is finished. Controlling the reaction temperature of the system to be 50 ℃ continuously, adjusting the reaction pH of the system to be 7.0 by ammonia water, and continuously stirring for 2 hours;
step S3: centrifugally washing the material in the step S2 by pure water, controlling the total solid-to-liquid ratio to be 1:5kg/L, centrifugally dehydrating, and vacuum drying at 110 ℃;
step S6: and (3) preserving heat of the material in the step (S3) for 0.5h at 300 ℃ and preserving heat of the material for 1h at 650 ℃ to obtain the anhydrous cobalt phosphate.
From fig. 4, the cobalt phosphate precursor has a lamellar morphology, the particle size distribution is uniform throughout, and no obvious ultra-large lamellar morphology exists.
Comparative example 1:
step S1: preparing a cobalt sulfate solution with the concentration of 1mol/L and a phosphoric acid solution with the concentration of 10mol/L for later use;
step S2: taking aqueous solution with pH of 6.0 adjusted by phosphoric acid as base solution, wherein the addition amount of the base solution is 50% of the total volume of the reaction kettle, controlling the reaction temperature of the system to be 30 ℃, and controlling the stirring linear speed to be 5m/s. And (3) adding the cobalt sulfate solution, the phosphoric acid solution and ammonia water (the mass percent of ammonia is 25-28%) into a reaction kettle in parallel, wherein the feeding amount of the cobalt sulfate solution is 250mL/min, the feeding speed of the phosphoric acid solution is 16.7mL/min, the pH of the ammonia water in the reaction process is controlled to be 9.0, and the total feeding time is 1h. Stirring for 0.5h after the feeding is finished;
step S3: centrifugally washing the material in the step S2 by pure water, controlling the total solid-to-liquid ratio to be 1:10kg/L, centrifugally dehydrating, and vacuum drying at 110 ℃;
step S6: and (3) preserving heat of the material in the step (S3) for 1h at 200 ℃ and preserving heat for 4h at 550 ℃ to obtain the anhydrous cobalt phosphate.
From fig. 5 and 6, the cobalt phosphate has a flaky morphology, the flaky layers are thicker, the particle size distribution is not uniform, and a part of oversized flaky morphology exists. XRD of fig. 7 shows that the precursor before calcination is a mixture of cobalt phosphate octahydrate and cobalt ammonium phosphate, and the precursor after calcination is an anhydrous cobalt phosphate structure.
Comparative example 2:
step S1: preparing a cobalt sulfate solution with the concentration of 1mol/L and a phosphoric acid solution with the concentration of 10mol/L for later use;
step S2: 15L of 1mol/L cobalt sulfate solution is used as a base solution, the reaction temperature of the system is controlled to be 30 ℃, and the stirring linear speed is controlled to be 5m/s. And (3) adding the phosphoric acid solution and ammonia water (the mass percentage of ammonia is 25-28%) into the reaction kettle in parallel, wherein the feeding speed of the phosphoric acid solution is 16.7mL/min, the pH of the ammonia water in the reaction process is controlled to be 6.0, and the total feeding time is 1h. Stirring is continued for 10min after the end of feeding. The reaction temperature of the system is controlled to be 30 ℃, the reaction pH of the ammonia water is adjusted to be 9.0, and the stirring is continued for 0.5h;
step S3: centrifugally washing the material in the step S2 by pure water, controlling the total solid-to-liquid ratio to be 1:10kg/L, centrifugally dehydrating, and vacuum drying at 110 ℃;
step S6: and (3) preserving heat of the material in the step (S3) for 1h at 200 ℃ and preserving heat for 4h at 550 ℃ to obtain the anhydrous cobalt phosphate.
As seen from fig. 8, the cobalt phosphate precursor mainly has a plate-like morphology, but the morphology and the particle size distribution are not uniform, and a flower-like morphology formed by partial plate intercalation exists.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (9)
1. The preparation method of the flaky cobalt phosphate is characterized by comprising the following steps of:
s1, preparing a cobalt salt solution and a phosphoric acid aqueous solution for later use;
s2, taking a phosphoric acid aqueous solution with a certain concentration as a base solution, flowing the soluble cobalt salt solution, the phosphoric acid aqueous solution and ammonia water prepared in the step S1 into a reaction kettle, reacting, controlling the pH value of a reaction system to be 4.0-6.0, continuing stirring for reaction time t1 after the feeding of the soluble cobalt salt solution and the phosphoric acid aqueous solution is finished, adjusting the inflow of the ammonia water to adjust the pH value of the reaction system to be 7.0-9.0, and stirring for reaction time t2; t1 is 10-30 min; t2 is 0.5-2 h; the feeding amount of the cobalt salt solution is 250-500 mL/min; the feeding amount of the phosphoric acid solution is 16.7-153.3 mL/min;
and S3, washing and drying the obtained material, and then calcining at high temperature to obtain the flaky cobalt phosphate.
2. The method for preparing the flaky cobalt phosphate according to claim 1, wherein in the step S2, the adding amount of the base solution accounts for 10-50% of the total volume of the reaction kettle, and the pH value of the base solution is 4.0-6.0.
3. The method of producing a cobalt phosphate sheet according to claim 1, wherein in the step S2, the reaction temperature is 30 to 50℃and the stirring line speed is 5 to 11m/S.
4. The method for preparing a cobalt phosphate sheet according to claim 1, wherein in the step S2, the feeding time of the cobalt salt solution and the phosphoric acid aqueous solution is 0.5 to 1h.
5. The method for preparing the flaky cobalt phosphate according to any one of claims 1 to 4, wherein the mass percentage of ammonia in the aqueous ammonia used is 25 to 28%.
6. The method for preparing a cobalt phosphate sheet according to any one of claims 1 to 4, wherein in step S3, the high-temperature calcination is: the temperature is kept for 0.5 to 1 hour at 200 to 300 ℃ and then is kept for 1 to 4 hours at 550 to 650 ℃.
7. The method for preparing the flaky cobalt phosphate according to any one of claims 1 to 4, wherein the cobalt salt is one or more of cobalt sulfate, cobalt chloride, cobalt nitrate and cobalt acetate.
8. The method for producing a cobalt phosphate sheet according to any one of claims 1 to 4, wherein in step S1, the concentration of the cobalt salt solution is 1.0 to 2.0mol/L; the concentration of the phosphoric acid aqueous solution is 5-10 mol/L.
9. The method for producing a cobalt phosphate sheet according to any one of claims 1 to 4, wherein in step S3, pure water is used as a cleaning agent for the washing; the consumption of the washing water is controlled to be 1:5-10 kg/L of total solid-liquid ratio; the drying is vacuum drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211466835.7A CN115535988B (en) | 2022-11-22 | 2022-11-22 | Preparation method of flaky cobalt phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211466835.7A CN115535988B (en) | 2022-11-22 | 2022-11-22 | Preparation method of flaky cobalt phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115535988A CN115535988A (en) | 2022-12-30 |
| CN115535988B true CN115535988B (en) | 2023-10-24 |
Family
ID=84720605
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211466835.7A Active CN115535988B (en) | 2022-11-22 | 2022-11-22 | Preparation method of flaky cobalt phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115535988B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104269528A (en) * | 2014-09-05 | 2015-01-07 | 中信国安盟固利电源技术有限公司 | Preparation method of cobalt phosphate powder material |
| CN108597896A (en) * | 2018-06-25 | 2018-09-28 | 金华职业技术学院 | A kind of preparation method and application of the cobalt phosphate nanometer sheet of Leaves'Shape |
| CN110600732A (en) * | 2019-09-07 | 2019-12-20 | 中南大学 | Preparation method of polyanion negative electrode material cobalt pyrophosphate |
| CN112390237A (en) * | 2021-01-21 | 2021-02-23 | 金驰能源材料有限公司 | Preparation method of nano-structure iron phosphate |
| CN112624079A (en) * | 2021-01-27 | 2021-04-09 | 金驰能源材料有限公司 | Preparation method of spherical iron phosphate |
| CN112938918A (en) * | 2019-12-10 | 2021-06-11 | 湖南杉杉能源科技股份有限公司 | Preparation method of cobalt phosphate powder material |
-
2022
- 2022-11-22 CN CN202211466835.7A patent/CN115535988B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104269528A (en) * | 2014-09-05 | 2015-01-07 | 中信国安盟固利电源技术有限公司 | Preparation method of cobalt phosphate powder material |
| CN108597896A (en) * | 2018-06-25 | 2018-09-28 | 金华职业技术学院 | A kind of preparation method and application of the cobalt phosphate nanometer sheet of Leaves'Shape |
| CN110600732A (en) * | 2019-09-07 | 2019-12-20 | 中南大学 | Preparation method of polyanion negative electrode material cobalt pyrophosphate |
| CN112938918A (en) * | 2019-12-10 | 2021-06-11 | 湖南杉杉能源科技股份有限公司 | Preparation method of cobalt phosphate powder material |
| CN112390237A (en) * | 2021-01-21 | 2021-02-23 | 金驰能源材料有限公司 | Preparation method of nano-structure iron phosphate |
| CN112624079A (en) * | 2021-01-27 | 2021-04-09 | 金驰能源材料有限公司 | Preparation method of spherical iron phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115535988A (en) | 2022-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106299347B (en) | Nickel cobalt aluminium ternary precursor and preparation method thereof and the positive electrode prepared and method | |
| CN111547780B (en) | Metal vanadate compound co-doped high-nickel ternary precursor and preparation method thereof | |
| CN106159254B (en) | Nano-sheet ternary or rich lithium manganese base solid solution positive electrode material precursor preparation method | |
| CN113562711B (en) | Ferric phosphate and preparation method and application thereof | |
| CN101269849A (en) | High-density spherical lithium nickel cobalt manganese oxygen and method for preparing the same | |
| CN109422297A (en) | Regulate and control the method for nucleation in a kind of nickel cobalt manganese presoma crystallization process | |
| CN108383171B (en) | Rapid preparation method of transition metal hydroxide nanoparticles | |
| CN108059182B (en) | Preparation method of rare earth layered hydroxide nanosheet and sol thereof | |
| CN106564867A (en) | Method for preparing iron phosphate material by adding reducing organic matters | |
| CN109904402A (en) | A kind of lithium-rich manganese base material and its preparation and application | |
| CN108539161B (en) | Preparation method of olive-shaped lithium manganese phosphate with prismatic protrusions on surface | |
| CN110504447A (en) | A kind of nickel cobalt manganese presoma of Fluorin doped and the preparation method and application thereof | |
| CN114195204B (en) | High sphericity manganese-rich carbonate precursor and preparation method and application thereof | |
| CN104478699A (en) | Preparation method of high-purity superfine cobalt oxalate powder | |
| CN1964103A (en) | A method to manufacture precursor of nickel-cobalt-lithium-manganese-oxide of lithium ion cell anode material | |
| CN103832991A (en) | Preparation method of iron phosphate nano material | |
| CN110817830A (en) | Method for preparing lithium iron phosphate electrode material from guanidino raw material | |
| CN108511724B (en) | Sol-gel assisted supercritical CO2Method for preparing lithium manganese iron phosphate by drying | |
| CN106517259A (en) | Spherical lithium carbonate and preparation method thereof | |
| CN115535988B (en) | Preparation method of flaky cobalt phosphate | |
| CN113753872A (en) | Comprehensive utilization method of iron-containing minerals | |
| CN109775734A (en) | A kind of preparation method of low specific surface area basic magnesium carbonate | |
| CN114988383B (en) | Efficient preparation method of battery-grade ferric phosphate | |
| CN110492060B (en) | Preparation method of nano-micro grade lithium manganese phosphate/carbon composite anode material | |
| CN113184823B (en) | Method for preparing cobalt nickel phosphate microsphere material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |