CN112142113A - Preparation method of spherical ammonium manganese vanadate particles - Google Patents
Preparation method of spherical ammonium manganese vanadate particles Download PDFInfo
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- CN112142113A CN112142113A CN202011048305.1A CN202011048305A CN112142113A CN 112142113 A CN112142113 A CN 112142113A CN 202011048305 A CN202011048305 A CN 202011048305A CN 112142113 A CN112142113 A CN 112142113A
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- ammonium
- vanadate particles
- manganese vanadate
- ammonium manganese
- spherical ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/006—Compounds containing, besides manganese, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a preparation method of spherical ammonium manganese vanadate particles. The invention aims to solve the technical problem of providing a preparation method of spherical ammonium manganese vanadate particles with short process and low cost. The method comprises the following steps: and (3) taking the calcified roasted vanadium leaching solution, adjusting the pH value to 1.8-2.2, adding ammonium chloride, uniformly stirring, and drying by adopting a spray dryer to obtain spherical ammonium manganese vanadate particles. The method shortens the process flow, reduces the production cost, and the prepared product has high sphericity and uniform particle size of 1-10 mu m.
Description
Technical Field
The invention belongs to the technical field of inorganic chemical industry, and particularly relates to a preparation method of spherical ammonium manganese vanadate particles.
Background
The ammonium manganese vanadate is a precursor of vanadium pentoxide and can be used as a positive electrode material of a lithium ion battery, the existing method for preparing the vanadium pentoxide precursor is a solution coprecipitation method, and the method has the defect that the prepared vanadium pentoxide precursors are different and uneven in appearance.
Patent document CN1369435 discloses a method for preparing spherical vanadium pentoxide and lithium vanadate as positive electrode material of lithium ion battery, which uses NH4VO3Melting at high temperature, and quenching in deionized water to form V2O5Sol is prepared into spherical V through spray drying2O5Sol powder is subjected to heat treatment to obtain the Li1+ xV ball3O8. The method has complicated process, involves heating to molten state at high temperature, taking out sample at high temperature, and directly putting into cold water to form V2O5Sol, spray drying to obtain spherical V2O5The method has the advantages of long flow, complex process, low process realizability, high risk, easy pipeline blockage and spray nozzle blockage of the sol in the spray drying process, and low yield.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of spherical ammonium manganese vanadate particles with short process and low cost.
The technical scheme adopted by the invention for solving the technical problems is to provide a preparation method of spherical ammonium manganese vanadate particles. The method comprises the following steps: and (3) taking the calcified roasted vanadium leaching solution, adjusting the pH value to 1.8-2.2, adding ammonium chloride, uniformly stirring, and drying by adopting a spray dryer to obtain spherical ammonium manganese vanadate particles.
In the preparation method of the spherical ammonium manganese vanadate particles, the calcified roasted vanadium leaching solution contains 15-20 g/L of vanadium, 8-10 g/L of manganese, 10-12 g/L of calcium, 5-8 g/L of iron, 0.2-0.5 g/L of phosphorus and 0.5-2 g/L of silicon.
Further, dilute hydrochloric acid solution with the volume fraction of 50% is adopted to adjust the pH value of the calcification roasting vanadium leaching solution.
Further, the adding amount of the ammonium chloride is controlled according to the ammonium adding coefficient of 2.3-2.8. The ammonium addition coefficient is the molar ratio of ammonium ions to vanadium ions.
Further, after adding ammonium chloride, the mixture was stirred for 15 minutes by a magnetic stirrer at a stirring rate of 300 rpm.
Further, the feeding speed is 400mL/min, the inlet temperature is 200-220 ℃, and the outlet temperature is 55-75 ℃ when the spray dryer is used for drying.
The invention has the beneficial effects that:
the method takes vanadium-containing leaching solution as raw material, adopts spray drying, and can prepare V2O5Front ofThe precursor ammonium manganese vanadate can complete three procedures of hydrolysis, spherical forming and dehydration in one step, thereby shortening the process flow, avoiding the need of wastewater treatment and reducing the production cost. The invention is not easy to block the pipeline and the spray nozzle in the preparation process, and the yield is high. The product prepared by the method has high sphericity and uniform particle size of 1-10 μm.
Detailed Description
Specifically, the invention provides a preparation method of spherical ammonium manganese vanadate particles. The method comprises the following steps: taking calcified roasting vanadium leachate with vanadium concentration of 15-20 g/L, adjusting the pH value of the calcified roasting vanadium leachate to 1.8-2.2 by adopting a dilute hydrochloric acid solution with volume fraction of 50%, adding ammonium chloride, stirring for 15 minutes by adopting a magnetic stirrer at the rotating speed of 300 revolutions per minute, drying by adopting a spray dryer, continuously stirring feed liquid by using the magnetic stirrer after spraying starts at the rotating speed of 300 revolutions per minute, feeding by using a peristaltic pump of the spray dryer at the feeding speed of 400mL/min, the inlet temperature of 200-220 ℃, and the outlet temperature of 55-75 ℃, thus obtaining the spherical manganese ammonium vanadate particles.
In order to facilitate the formation of ammonium manganese vanadate, the pH value of the calcification roasting vanadium leaching solution is controlled to be 1.8-2.2.
In order to improve the balling rate of the ammonium manganese vanadate particles, the feeding speed of the spray dryer is controlled to be 400mL/min, the inlet temperature is 200-220 ℃, and the outlet temperature is 55-75 ℃.
The innovation point of the invention is that the V is prepared by using calcified roasted vanadium-containing leaching solution as a raw material and adopting spray drying2O5The precursor manganese ammonium vanadate completes three procedures of hydrolysis, spherical forming and dehydration in one procedure, greatly shortens the process flow and reduces the production cost.
The present invention will be further illustrated by the following specific examples.
Example 1
Taking 200mL of calcified roasted vanadium leachate containing 15g/L of vanadium, 8g/L of manganese, 10g/L of calcium, 6g/L of iron, 0.2g/L of phosphorus and 0.5g/L of silicon, adding a dilute hydrochloric acid solution with the volume fraction of 50% to adjust the pH value to 1.8, adding 12.3g of ammonium chloride, calculating the ammonium addition amount by the ammonium addition coefficient of 2.3, stirring for 15 minutes by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, continuing stirring the material liquid by using the magnetic stirrer after the beginning of injection at the rotating speed of 300 revolutions per minute, feeding by using a peristaltic pump for a spray dryer at the feeding speed of 400mL/min, at the inlet temperature of 200 ℃ and at the outlet temperature of 55 ℃, and injecting the material liquid to obtain spherical ammonium vanadate particles. The particle size is 2-8 μm.
Example 2
Taking 200mL of calcified roasted vanadium leachate containing 18g/L of vanadium, 9g/L of manganese, 11g/L of calcium, 7g/L of iron, 0.3g/L of phosphorus and 1g/L of silicon, adding a dilute hydrochloric acid solution with the volume fraction of 50% to adjust the pH value to 2.2, adding 12.3g of ammonium chloride, calculating the ammonium addition amount by the ammonium addition coefficient of 2.3, stirring for 15 minutes by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, continuing stirring the material liquid by using the magnetic stirrer after the injection is started at the rotating speed of 300 revolutions per minute, feeding by using a peristaltic pump for a spray dryer at the feeding speed of 400mL/min, at the inlet temperature of 220 ℃ and at the outlet temperature of 75 ℃, and injecting the material liquid to obtain spherical ammonium manganese vanadate particles. The particle size is 3-9 μm.
Example 3
Taking 200mL of calcified roasted vanadium leachate containing 20g/L of vanadium, 10g/L of manganese, 12g/L of calcium, 8g/L of iron, 0.5g/L of phosphorus and 2g/L of silicon, adding a dilute hydrochloric acid solution with the volume fraction of 50% to adjust the pH value to 1.8, adding 20g of ammonium chloride, calculating the ammonium addition amount by the ammonium addition coefficient of 2.8, stirring for 15 minutes by using a magnetic stirrer at the rotating speed of 300 revolutions per minute, continuing stirring the material liquid by using the magnetic stirrer after the injection starts, at the rotating speed of 300 revolutions per minute, feeding by using a peristaltic pump for a spray dryer, at the feeding speed of 400mL/min, at the inlet temperature of 200 ℃ and at the outlet temperature of 55 ℃, and injecting the material liquid to obtain spherical ammonium manganese vanadate particles. The particle size is 2 to 6 μm.
Claims (6)
1. The preparation method of the spherical ammonium manganese vanadate particles is characterized by comprising the following steps of: the method comprises the following steps: and (3) taking the calcified roasted vanadium leaching solution, adjusting the pH value to 1.8-2.2, adding ammonium chloride, uniformly stirring, and drying by adopting a spray dryer to obtain spherical ammonium manganese vanadate particles.
2. The method of preparing spherical ammonium manganese vanadate particles according to claim 1, wherein: the calcified roasted vanadium leaching solution contains 15-20 g/L vanadium, 8-10 g/L manganese, 10-12 g/L calcium, 5-8 g/L iron, 0.2-0.5 g/L phosphorus and 0.5-2 g/L silicon.
3. The method of preparing spherical ammonium manganese vanadate particles according to claim 1 or 2, characterized in that: and (3) adjusting the pH value of the calcified roasted vanadium leaching solution by adopting a dilute hydrochloric acid solution with the volume fraction of 50%.
4. The method for preparing spherical ammonium manganese vanadate particles according to any one of claims 1 to 3, wherein: the adding amount of the ammonium chloride is controlled according to the ammonium adding coefficient of 2.3-2.8.
5. The method for preparing spherical ammonium manganese vanadate particles according to any one of claims 1 to 4, wherein the method comprises the following steps: after the addition of ammonium chloride, the mixture was stirred for 15 minutes with a magnetic stirrer at a stirring rate of 300 revolutions per minute.
6. The method for preparing spherical ammonium manganese vanadate particles according to any one of claims 1 to 5, wherein: the feeding speed when the spray dryer is adopted for drying is 400mL/min, the inlet temperature is 200-220 ℃, and the outlet temperature is 55-75 ℃.
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Citations (5)
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| GB555127A (en) * | 1941-01-24 | 1943-08-05 | Celluloid Corp | Nacreous compositions and plastics decorated therewith |
| US3595755A (en) * | 1967-03-10 | 1971-07-27 | Merck Ag E | Detection of hydrogen peroxide |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
| DE102014114293A1 (en) * | 2014-10-01 | 2016-04-07 | Bundesrepublik Deutschland, Vertreten Durch Den Bundesminister Für Wirtschaft Und Energie, Dieser Vertreten Durch Den Präsidenten Der Bundesanstalt Für Materialforschung Und -Prüfung (Bam) | Weather resistant and transparent enamel colors for stained glass |
| WO2016205003A1 (en) * | 2015-06-16 | 2016-12-22 | Conair Corporation | Method for removing a tatoo |
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2020
- 2020-09-29 CN CN202011048305.1A patent/CN112142113A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB555127A (en) * | 1941-01-24 | 1943-08-05 | Celluloid Corp | Nacreous compositions and plastics decorated therewith |
| US3595755A (en) * | 1967-03-10 | 1971-07-27 | Merck Ag E | Detection of hydrogen peroxide |
| CN104649253A (en) * | 2013-11-18 | 2015-05-27 | 国家纳米科学中心 | Preparing methods of porous graphene and porous graphene film |
| DE102014114293A1 (en) * | 2014-10-01 | 2016-04-07 | Bundesrepublik Deutschland, Vertreten Durch Den Bundesminister Für Wirtschaft Und Energie, Dieser Vertreten Durch Den Präsidenten Der Bundesanstalt Für Materialforschung Und -Prüfung (Bam) | Weather resistant and transparent enamel colors for stained glass |
| WO2016205003A1 (en) * | 2015-06-16 | 2016-12-22 | Conair Corporation | Method for removing a tatoo |
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| 王新翠等: "壳聚糖/Ti-W-V-Mn基金属氧化物复合脱硝催化剂的制备及性能研究", 《化工新型材料》 * |
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Application publication date: 20201229 |