Production device of nano ferromanganese phosphate

Abstract

The utility model discloses a production device of nano ferromanganese phosphate. The production device comprises a mixer, a grinder, a filter, a dryer and a calcining furnace which are connected in sequence, the mixer is used for mixing the phosphoric acid aqueous solution and the ferromanganese oxide; the grinder is used for grinding a mixed solution of a phosphoric acid aqueous solution and a ferromanganese oxide and enabling the phosphoric acid aqueous solution and the ferromanganese oxide to react; the filter is used for filtering slurry obtained after grinding; the dryer is used for drying a solid obtained after the slurry is filtered; and the calcining furnace is used for calcining the dried solid. Preferably, the filter is also used for filtering the slurry obtained after grinding and then cleaning the slurry; preferably, a plurality of sanding beads are arranged in the grinder. According to the production device, the ferromanganese phosphate material can be synthesized by a one-step method, and the corresponding preparation method can be basically completed mechanically, so that the production cost is low, industrialization is easy, and nano-porous ferromanganese phosphate can be prepared.

Description

Technical Field

[0001] The utility model relates to a production device for nano-manganese ferrophosphate. Background Art

[0002] In recent decades, nanomaterials and porous materials are functional materials with special structures. They have played a unique role and value in many application fields such as photocatalysis, solar cells, electromagnetism, optics, etc., and have attracted the attention of scientific researchers. Ferromanganese phosphate materials can be used as phosphating agents to prevent rust and corrosion of steel products; they can also be used as ion exchangers, sensors, adsorbents, magnetic materials, etc., and are very important non-metallic inorganic materials. In addition, ferromanganese phosphate can also be used as an important precursor material for manganese-iron phosphate positive electrode materials in lithium-ion batteries. Since manganese and iron have a uniform mixing degree at the atomic level in ferromanganese phosphate materials, when used to prepare manganese-iron phosphate positive electrode materials, the distribution of manganese-iron metal elements in the positive electrode materials is also uniformly distributed at the atomic level, which is beneficial to improve the rate performance and cycle stability of manganese-iron phosphate lithium-ion batteries, and improve voltage drop and manganese dissolution.

[0003] Chinese patent CN111908442A discloses a method for preparing ferromanganese phosphate, which uses manganese dioxide, ferrous oxalate and phosphoric acid to react in the presence of a reducing agent to obtain (Mn 1-x Fe x ) a PO4·H2O crystals, and then filtered, washed, and sintered at high temperature to obtain amorphous (Mn 1-x Fe x ) a PO4 powder, a reducing agent needs to be introduced during the preparation process of this method, and heating is required during the reaction process; the prepared ferromanganese phosphate material has a large particle size of micron level, and has a high particle density and a non-porous structure.

[0004] When preparing ferromanganese phosphate in the prior art, oxidation-precipitation method, reduction-precipitation method or hydrothermal method is usually adopted, but these preparation methods require relatively complex supporting production equipment, high production cost, and difficult to industrialize, and the particle size of ferromanganese phosphate prepared by these methods is usually micrometer level, the particle density is high, and it is usually a non-porous structure. The prior art lacks a production device that can be used for industrial preparation of ferromanganese phosphate with a size of less than 50nm and a porous structure. Utility Model Content

[0005] In order to overcome the defects of the prior art, the purpose of the utility model is to provide an improved production device of nano-manganese ferrophosphate, which has a simple structure, low production cost, and is easy to industrialize. By using the production device, porous manganese ferrophosphate with a particle size of less than 50nm can be prepared.

[0006] In order to solve the above problems, the utility model provides the following solutions:

[0007] A production device for nano-manganese ferrophosphate, comprising a mixer, a grinder, a filter, a dryer and a calcining furnace connected in sequence; the mixer is used to mix a phosphoric acid aqueous solution and manganese iron oxide; the grinder is used to grind the mixed solution of the phosphoric acid aqueous solution and the manganese iron oxide and make the two react; the filter is used to filter the slurry obtained after grinding; the dryer is used to dry the solid obtained after filtering the slurry; and the calcining furnace is used to calcine the dried solid.

[0008] In the present utility model, the mixer can be a conventional mixer in the chemical industry, as long as it can fully mix the phosphoric acid aqueous solution and the manganese iron oxide. For example, the mixer can be a slurry mixing barrel commonly used in the chemical industry. The grinder can be a conventional grinder in the chemical industry, such as a grinder commonly used in the chemical industry, which is used to reduce the particle size of the manganese iron oxide and promote phosphoric acid and manganese iron oxide to fully react to generate a slurry containing manganese iron phosphate monohydrate. The filter can be a conventional filter in the chemical industry, as long as it can filter the slurry containing manganese iron phosphate monohydrate after grinding and separate the solid and liquid in the slurry. The dryer can be a conventional dryer in the chemical industry, such as a flash evaporator, etc., which is used to dry the filter residue solid after the slurry is filtered to obtain a manganese iron phosphate monohydrate solid. The specific structure of the calcining furnace is not particularly limited. The calcining equipment commonly used in the chemical industry, such as a rotary kiln, etc., can be used. Its function is to calcine the manganese iron phosphate monohydrate solid to generate a nano-level manganese iron phosphate target product.

[0009] In some embodiments, the filter is also used to wash the slurry obtained after grinding after filtering. When phosphoric acid reacts with manganese iron oxide, phosphoric acid is usually used in an excess amount of molar equivalent ratio. After filtering the slurry, further washing in the filter can remove excess phosphoric acid. Filters conventionally used in the chemical industry can usually achieve the function of washing. For example, the filter is usually connected to a water pipe, and water can be passed from the water pipe to wash the material.

[0010] In some embodiments, the mixer includes a mechanical stirrer. The mechanical stirrer can improve the mixing effect of the phosphoric acid aqueous solution and the manganese iron oxide. Conventional mechanical stirring equipment in the chemical industry can be used.

[0011] In some embodiments, the particle size of the nano-manganese ferrophosphate is less than 50 nm. In a grinder, the phosphoric acid aqueous solution and the manganese iron oxide react while grinding, so that the size of the obtained manganese ferrophosphate nanoparticles can be reduced.

[0012] In some embodiments, a plurality of sanding beads are disposed in the grinder.

[0013] In some embodiments, the sanding beads are made of zirconium oxide.

[0014] In some embodiments, the sand grinding beads are spherical and have a diameter of 0.1-5.0 mm. The use of the sand grinding beads can improve the grinding effect of the two in the grinder, which is conducive to reducing the size of the manganese iron phosphate nanomaterial.

[0015] In some embodiments, the grinder is used to grind the particles in the mixed solution to a particle size of less than 100 nm.

[0016] In some embodiments, the production device further comprises a power pump disposed between the mixer and the grinder, and between the grinder and the filter. The use of a power pump to transport materials such as slurry can increase the material transport rate and improve production efficiency.

[0017] In some embodiments, the production device further includes a filtrate recovery device for recovering the filtrate obtained after filtering the filter, and the filtrate recovery device is connected to the filter and the mixer respectively. The filtrate recovery device can recover the liquid in the slurry, such as phosphoric acid aqueous solution, and further react in the mixer after recovery, which is conducive to improving the economic benefits of ferromanganese phosphate production.

[0018] In some embodiments, the production device further includes a power pump disposed between the filter and the filtrate recovery device, and the filter and the power pump, the power pump and the filtrate recovery device, and the filtrate recovery device and the mixer are connected by pipelines. The use of a power pump to transport materials such as slurry can increase the material transport rate and improve production efficiency.

[0019] In some embodiments, the dryer is a flash evaporator, which can be a conventional flash evaporator in the chemical industry.

[0020] In some embodiments, the calcining furnace is a rotary kiln, which can be a conventional rotary kiln in the chemical industry.

[0021] In some embodiments, the mixer and the grinder, the grinder and the filter, and the filter and the dryer are connected by pipelines, and the dryer and the calciner are connected by a powder conveyor belt. Materials in slurry or liquid state are transported by pipelines, and materials such as powders are transported by powder conveyor belts.

[0022] In some embodiments, the production device further comprises a material collecting bucket connected to the calcining furnace, wherein the material collecting bucket is connected to the calcining furnace via a powder conveyor belt. The material collecting bucket can temporarily store the ferromanganese phosphate nanomaterial product, and transfer the product after a certain amount of the product is collected.

[0023] The beneficial effects of the utility model are:

[0024] The nanometer ferromanganese phosphate production device of the utility model can synthesize ferromanganese phosphate material by a one-step method, and the corresponding preparation method can be basically completed by machinery, which can reduce production costs and facilitate industrialization.

[0025] By adjusting the size of the sand beads in the grinder, the size of the obtained manganese iron phosphate nanoparticle material can be controlled.

[0026] By utilizing the production device of the utility model, ferromanganese phosphate with a particle size of less than 50nm can be prepared. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a schematic diagram of the structure of a production device for nano-manganese ferrophosphate;

[0028] Among them, 1-mixer, 2-mechanical agitator, 3-power pump, 4-grinder, 5-filter, 6-dryer, 7-calcining furnace, 8-collecting barrel, 9-filtrate recovery device, 10-powder conveyor belt, 11-pipeline.

[0029] The present invention will be further described below in conjunction with the accompanying drawings and specific implementation methods. DETAILED DESCRIPTION

[0030] The utility model specifically provides a production device for nano-manganese ferrophosphate. The innovation of the production device is to set a mixer for mixing phosphoric acid aqueous solution and manganese iron oxide, and then transport the mixture of the two to a grinder for grinding and dispersing the two, and set a filter for filtering the slurry obtained by grinding after the grinder, and set a dryer for drying the solid obtained by filtering after the filter, and set a calcining furnace for calcining the above solid after the dryer. With the production device, the production of manganese ferrophosphate can be completed mechanically, and manganese ferrophosphate with a nanoporous structure can be obtained, which reduces the production cost of manganese ferrophosphate and enables the production method of manganese ferrophosphate to be industrialized on a large scale.

[0031] The production device of nano-manganese ferrophosphate of the utility model can be specifically implemented as follows:

[0032] The production device includes a mixer 1, a grinder 4, a filter 5, a dryer 6 and a calciner 7 connected in sequence; the mixer 1 is used to mix the phosphoric acid aqueous solution and the manganese iron oxide; the grinder 4 is used to grind the mixed solution of the phosphoric acid aqueous solution and the manganese iron oxide and make the two react fully; the filter 5 is used to filter the slurry obtained after grinding, and the filter 5 is also used to wash the slurry obtained after grinding after filtering, for example, a water pipe can be connected to the filter 5, and water can be passed from the water pipe to the filter 5 to wash the filtered slurry; the dryer 6 is used to dry the solid obtained after the slurry is filtered; the calciner 7 is used to calcine the dried solid. The mixer 1, the grinder 4, the filter 5, the dryer 6 and the calciner 7 can all adopt the mixers, grinders, filters, dryers and calciners commonly used in the chemical industry, for example, the dryer can adopt a flash evaporator, and the calciner can adopt a rotary kiln. The mixer 1 includes a mechanical agitator 2. A plurality of sanding beads are arranged in the grinder 4. The sanding beads are made of zirconium oxide, are spherical, and have a diameter of 0.1-5.0 mm. The grinder 4 is used to grind the particles in the mixed solution to a particle size of less than 100 nm.

[0033] The production device further comprises a filtrate recovery device 9 for recovering the filtrate obtained after filtering by the filter 5 , and the filtrate recovery device 9 is connected to the filter 5 and the mixer 1 respectively.

[0034] A power pump 3 is provided between the mixer 1 and the grinder 4, between the grinder 4 and the filter 5, and between the filter 5 and the filtrate recovery device 9. The filter 5 and the power pump 3, the power pump 3 and the filtrate recovery device 9, the filtrate recovery device 9 and the mixer 1, the mixer 1 and the grinder 4, the grinder 4 and the filter 5, and the filter 5 and the dryer 6 are all connected by pipelines. The dryer 6 and the calcining furnace 7 are connected by a powder conveyor belt 10. A receiving barrel 8 connected to the rotary kiln is also provided after the rotary kiln, and the two are connected by a powder conveyor belt 10.

[0035] use Figure 1 An example of a production plant producing ferromanganese phosphate is shown below:

[0036] Concentrated phosphoric acid solution and deionized water are added to the mixer 1 in sequence, and the mixture is stirred evenly by a mechanical stirrer 2 to prepare a phosphoric acid aqueous solution with a mass concentration of 35%; a corresponding mass of micron-sized manganese iron oxide (molecular formula: (Mn 0.6 Fe 0.4 )3O4, purchased from Sichuan Qingyuan New Materials Co., Ltd., with an average particle size of 7 μm), was mechanically stirred in a mixer 1 for 12 hours to obtain a reaction mixture;

[0037] The reaction mixture is conveyed to the grinder 4 through the power pump 3 for grinding. The grinder 4 is provided with zirconium oxide grinding beads, which are spherical and have a diameter of 0.1-5 mm. After sand grinding for 1 hour, a dark green slurry is obtained. The slurry is conveyed to the filter 5 through the power pump 3 for filtration and cleaning. The solid obtained by filtration and cleaning is conveyed to the dryer 6 through the pipeline 11 for drying. The drying temperature is 100°C. After drying, dark green manganese iron phosphate monohydrate is obtained. At the same time, the filtrate obtained by filtration is conveyed to the filtrate recovery device 9 through the power pump 3. The filtrate recovered in the filtrate recovery device 9 is returned to the mixer 1 through the pipeline 11. The dried powder is conveyed to the calcining furnace 7 through the powder conveyor belt 10 for calcination. The calcination temperature is 400°C and the calcination time is 2 hours. A reddish brown nanoporous structure of manganese iron phosphate is obtained, which is conveyed to the receiving barrel 8 through the powder conveyor belt 10 for storage and collection.

[0038] According to characterization, the particle size of the nanoporous manganese iron phosphate is 40nm, with a mesoporous structure, the pore size is mainly distributed in the range of 3-5nm, and the specific surface area is 15m 2 / g, and the crystal phase is a monoclinic phase structure. The manganese iron phosphate is used to synthesize manganese iron phosphate lithium positive electrode material, and the obtained positive electrode material has excellent electrical properties.

[0039] The above disclosure is only the preferred embodiment of the present invention, which certainly cannot be used to limit the scope of rights of the present invention. Therefore, equivalent changes made according to the scope of the patent application of the present invention are still within the scope covered by the present invention.

Claims

1. A production device for nano-manganese ferrophosphate, characterized in that: The production device comprises a mixer, a grinder, a filter, a dryer and a calciner connected in sequence; the mixer is used to mix the phosphoric acid aqueous solution and the manganese iron oxide; the grinder is used to grind the mixed solution of the phosphoric acid aqueous solution and the manganese iron oxide and make the two react; the filter is used to filter the slurry obtained after grinding; The dryer is used to dry the solid obtained after filtering the slurry; The calciner is used to calcine the dried solid.

2. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The mixer includes a mechanical stirrer; and / or the filter is also used to clean the slurry obtained after grinding after filtering.

3. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The particle size of the nano-manganese ferrophosphate is less than 50 nm.

4. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: A plurality of sanding beads are arranged in the grinder.

5. The production device of nano-manganese ferrophosphate according to claim 4, characterized in that: The sanding beads are made of zirconium oxide; and / or the sanding beads are spherical and have a diameter of 0.1-5.0 mm.

6. The production device of nano-manganese ferrophosphate according to claim 1, 4 or 5, characterized in that: The grinder is used to grind the particles in the mixed solution to a particle size of less than 100 nm.

7. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The production device further comprises a power pump arranged between the mixer and the grinder, and between the grinder and the filter.

8. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The production device also includes a filtrate recovery device for recovering the filtrate obtained after filtering by the filter, and the filtrate recovery device is connected to the filter and the mixer respectively.

9. The production device of nano-manganese ferrophosphate according to claim 8, characterized in that: The production device also includes a power pump arranged between the filter and the filtrate recovery device. The filter and the power pump, the power pump and the filtrate recovery device, and the filtrate recovery device and the mixer are connected through pipelines.

10. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The dryer is a flash evaporator; and / or the calcining furnace is a rotary kiln.

11. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The mixer and the grinder, the grinder and the filter, and the filter and the dryer are connected through pipelines, and the dryer and the calcining furnace are connected through a powder conveyor belt.

12. The production device of nano-manganese ferrophosphate according to claim 1, characterized in that: The production device also includes a material receiving barrel connected to the calcining furnace, and the material receiving barrel is connected to the calcining furnace through a powder conveyor belt.

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