CN215279880U - Metal lithium powder production device - Google Patents
Metal lithium powder production device Download PDFInfo
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- CN215279880U CN215279880U CN202121156207.XU CN202121156207U CN215279880U CN 215279880 U CN215279880 U CN 215279880U CN 202121156207 U CN202121156207 U CN 202121156207U CN 215279880 U CN215279880 U CN 215279880U
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Abstract
Disclosed is a device for producing lithium metal powder. This lithium metal powder apparatus for producing includes: the pressure-resistant container comprises a container wall and an inner space limited by the container wall, wherein a feed inlet and a discharge opening are formed in the container wall, and a discharge valve and a pressurization opening are formed in the discharge opening; and a baffle plate located outside the pressure vessel and arranged opposite to the discharge port. The production device of the metal lithium powder can efficiently prepare the metal lithium powder with small particle size and high purity.
Description
Technical Field
The utility model relates to a metal processing and production technical field especially relate to metal lithium powder apparatus for producing.
Background
The traditional production method of the lithium metal powder has two types: the first method is a melt emulsification method adopted by FMC company, the surface of the lithium metal powder prepared by the method is provided with a passivation layer, the purity of the lithium metal powder is low, and the lithium metal powder is not easy to prepare in large batch; the second method is a dry lithium powder preparation process of Tianjin lithium industry Co., Ltd, namely, metal lithium is dripped on an ultrasonic probe, and molten lithium is crushed by ultrasonic waves, but the metal lithium powder prepared by the method has large particles and is easy to cause discharge port blockage in the preparation process. Therefore, there is a need to develop a new lithium metal powder preparation process and apparatus to realize large-scale industrial preparation of lithium metal powder with small diameter and high purity.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a can high-efficient device of preparing the metal lithium powder that the particle diameter is little, purity is high.
The purpose of the utility model can be realized by the following technical scheme.
A lithium metal powder production apparatus, comprising:
a pressure resistant vessel comprising:
a container wall having disposed thereon:
a feed inlet;
the discharging opening is provided with a discharging valve; and
a pressure port, and
an interior space defined by the container wall, an
And the baffle is positioned outside the pressure vessel and is opposite to the discharge opening.
In certain embodiments, the distance between the discharge opening and the baffle is from 1cm to 50 cm.
In certain embodiments, the discharge opening has an outlet diameter of 0.01mm to 5 mm.
In certain embodiments, the pressure-resistant container is further provided with a heating means and a heat-insulating means.
In certain embodiments, the heating means is disposed on the container wall and the insulating means is an insulating layer located on the outermost side of the container wall.
In certain embodiments, the pressure resistant vessel further comprises a pressure gauge disposed on the vessel wall.
In certain embodiments, the baffle surface is provided with a lithium phobic protective layer.
In certain embodiments, the lithium metal powder production apparatus further comprises a casing forming an enclosed space for accommodating the pressure-resistant container and the baffle.
In certain embodiments, the lithium metal powder production apparatus further comprises a temperature adjustment mechanism for adjusting a temperature of at least one of the baffle and the enclosed space.
In certain embodiments, the temperature adjustment mechanism comprises a coolant line disposed inside the baffle.
The technical scheme of the utility model one of following advantage has at least:
1. the utility model discloses a lithium powder apparatus for producing's is efficient, and the metal lithium powder particle diameter of preparation is little, and purity is high.
2. The particle size of the metal lithium powder is controllable.
Drawings
Fig. 1 is a schematic view of a lithium powder production apparatus according to the present invention.
Fig. 2 is a graph of particle size test data for examples and comparative examples of the present invention.
Description of reference numerals:
1. a pressure resistant vessel; 2. a feed inlet; 3. a discharge opening; 4. a discharge valve; 5. a pressurizing port; 6. a heating device; 7. a heat-insulating layer; 8. a pressure gauge; 9. baffle plate
Detailed Description
The following describes a specific embodiment of the present invention. It is to be understood that other various embodiments can be devised and modified by those skilled in the art in light of the teachings of this disclosure without departing from the scope or spirit of the invention. The following detailed description is, therefore, not to be taken in a limiting sense.
Fig. 1 is a schematic diagram of a lithium powder production device provided by the present invention. The production apparatus comprises a pressure-resistant vessel 1 and a baffle 9 in an enclosed space protected with an inert gas (e.g., high-purity argon gas, high-purity helium gas). The pressure-resistant container 1 comprises a container wall and an inner space limited by the container wall, a feed inlet 2 and a discharge opening 3 are arranged on the container wall, a discharge valve 4 and a pressurizing opening 5 are arranged on the discharge opening 3, and a pressure gauge 8 is arranged on the container wall in a preferred embodiment. Wherein, the feed inlet 2 is used for feeding solid lithium metal into the pressure vessel 1, the discharge outlet 3 is used for discharging the heated and melted lithium metal from the pressure vessel 1, and the pressurizing outlet 5 is used for applying pressure to the inside of the pressure vessel 1 so as to increase the pressure difference of the pressure vessel 1, so that the melted lithium metal is discharged from the discharge outlet 3 (forming jet flow) at a certain initial speed. The wall of the pressure-resistant vessel 1 may also be provided with heating means (e.g., heating wires) 6 and an insulating layer 7. The heating means 6 is for heating the metallic lithium in the pressure-resistant vessel 1, and the insulating layer 7 is located on the outermost side of the vessel wall for maintaining the internal temperature of the pressure-resistant vessel 1. The baffle 9 is located outside the pressure vessel 1 opposite to the discharge opening 3 so that the jet discharged from the discharge opening 3 can collide with the baffle 9.
The basic design idea of the lithium powder production method of the utility model is as follows: melting the lithium metal at high temperature, discharging the liquid lithium metal through a narrow outlet (discharge opening) in a jet form under a certain pressure difference, and colliding the lithium metal jet with a baffle (preferably fully cooling before collision) so as to crush the lithium metal into lithium metal powder with small diameter and high purity.
In the present invention, the lithium metal used as the raw material may be a purified lithium ingot, and the content of the lithium metal is 99%, preferably 99.9% or more. The lithium ingot preferably has a volume of about 1/3 to 2/3 of the inner space of the pressure-resistant container.
The temperature at which the metallic lithium is heated and melted in the pressure-resistant vessel 1 may be 180 ℃ to 3000 ℃, preferably 200 ℃ to 1000 ℃, more preferably 250 ℃ to 600 ℃. The internal pressure of the pressure-resistant vessel 1 may be 0.1MPa to 300MPa, preferably 1MPa to 100MPa, more preferably 10MPa to 50MPa, so that a sufficient pressure difference can be established between the inside and the outside of the pressure-resistant vessel 1. It is also possible to form or increase the injection pressure difference by forming a negative pressure outside the pressure-resistant container 1. The temperature of the molten lithium and the injection pressure difference provide energy for injecting the molten lithium liquid, and the larger the energy is, the larger the specific surface area of the lithium powder can be obtained, i.e., the lithium powder with a small diameter.
The size of the opening (ejection opening) of the discharge opening 3 for discharging the molten metallic lithium also affects the particle diameter of the obtained lithium powder. On one hand, the size of the ejection opening and the ejection pressure difference determine the ejection speed of the molten lithium liquid (and further the collision kinetic energy with the baffle), on the other hand, the size of the ejection opening has a certain influence on the energy release rate of the molten lithium, and when the ejection opening is large, the heat dissipation of the molten lithium ejected when the molten lithium is cooled is slow, so that the molten lithium is not suitable for obtaining spherical lithium powder with small particle size. Thus, the discharge opening diameter is generally from 0.01mm to 5mm, preferably from 0.1mm to 3 mm.
There is no particular requirement for the shape of the discharge opening 3 other than the size of the discharge opening. In general, the discharge opening 3 may have a straight tubular shape to facilitate the discharge of the molten lithium liquid as quickly as possible. In some cases, the opening direction (upward or downward) of discharge port 3 may also be designed to change the exit angle of the molten lithium liquid. The discharge opening may be tapered toward the discharge opening to increase the discharge speed of the molten lithium.
The injection distance of the molten lithium liquid influences the particle size and morphology of the obtained lithium powder. Generally, the smaller the ejection distance is, the smaller the diameter of the obtained lithium powder is (because the kinetic energy attenuation is reduced), but if the ejection distance is too small, the ejected lithium powder can be partially pulverized, but most of the crushed lithium liquid is easily adhered to each other or the ejected lithium liquid because the heat is not released yet, so that the lithium powder is agglomerated, and the appearance is not good. When the injection distance is long, the surface tension of the molten lithium becomes large, and the molten lithium is not easily broken to obtain lithium powder. Therefore, the distance between the discharge opening and the baffle plate should be appropriately set. Typically, the distance between the discharge opening and the baffle is from 1cm to 50cm, preferably from 1cm to 10 cm. In addition, in order to facilitate the energy release of the injected molten lithium, the baffle plate and the atmosphere can be provided with temperature reduction measures, for example, the temperature of the baffle plate and/or the atmosphere outside the pressure-resistant container is adjusted through a temperature adjusting mechanism. In some embodiments, the baffle is a thermostatic plate with a coolant line disposed therein.
To reduce the possibility of molten lithium liquid sticking to the baffle after colliding with the baffle, the baffle may have a lithium phobic design. For example, the baffle may be formed of a lithium-phobic material or a layer of lithium-phobic material may be formed on the surface of the baffle. As the lithium-phobic material, diamond, metal gallium, metal tungsten, or the like can be selected.
It should be noted that, since lithium metal is very sensitive to oxygen, moisture, etc. (especially at high temperature), all steps of the lithium powder production method of the present invention are carried out under the protection of inert atmosphere. For example, in a glove box under argon or helium protection.
Example 1:
the production apparatus shown in FIG. 1 was used to charge purified lithium ingots, the volume of which was about 1/3 to 2/3, into the pressure vessel. Sealing the pressure-resistant container, starting a heating wire to heat the pressure-resistant container, and carrying out heat preservation treatment after the temperature is raised to 300 ℃. Connecting pressurized inert gas from the pressurizing port, opening the valve to pressurize the pressure container, and maintaining the pressurizing pressure unchanged when the pressure gauge reaches 5 MPa. The position of the baffle is set, and the distance between the baffle and the discharge opening is guaranteed to be 10 cm. The discharge opening (diameter 1mm) was opened and the lithium liquid impacted the baffle and was broken into small particles. The obtained lithium powder particles were collected to be subjected to a laser particle size test to confirm the diameter of the lithium powder.
Example 2
The preparation was carried out as in example 1, varying the pressure difference to 20 MPa.
Example 3
The preparation was carried out as in example 1, varying the diameter of the injection opening to 0.1 mm.
Example 4
The preparation process was as in example 1, with the baffle plate being spaced 5cm from the discharge opening.
Comparative example 1
Lithium powder of FMC is commercially available.
The lithium powder was subjected to particle size measurement using a hundred-tex laser particle sizer (BT-9300LD) in a glove box protected by an inert atmosphere, and the results are shown in fig. 2. The particle size test data for each example is shown in table 1.
TABLE 1 particle size test data for each of the examples and comparative examples
| Sample (I) | D06 | D10 | D16 | D25 | D50 | D75 | D85 | D90 | D98 |
| Example 1 | 2.897 | 3.567 | 4.526 | 5.985 | 10.50 | 16.77 | 20.80 | 23.75 | 33.58 |
| Example 2 | 1.449 | 1.781 | 2.197 | 2.795 | 4.669 | 7.425 | 9.156 | 10.37 | 14.05 |
| Example 3 | 1.882 | 2.179 | 2.608 | 3.272 | 5.433 | 8.591 | 10.40 | 11.58 | 14.87 |
| Example 4 | 2.814 | 3.438 | 4.332 | 5.688 | 9.884 | 15.57 | 19.03 | 21.47 | 28.92 |
| Comparative example 1 | 3.296 | 4.204 | 5.533 | 7.526 | 13.63 | 23.20 | 29.95 | 35.07 | 51.02 |
Although the present invention has been disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the scope or spirit of the present invention, and the scope of the present invention is defined by the appended claims.
Claims (10)
1. A lithium metal powder production apparatus, characterized in that the apparatus comprises:
a pressure resistant vessel comprising:
a container wall having disposed thereon:
a feed inlet;
the discharging opening is provided with a discharging valve; and
a pressure port, and
an interior space defined by the container wall, an
And the baffle is positioned outside the pressure vessel and is opposite to the discharge opening.
2. The lithium metal powder production apparatus of claim 1, wherein the discharge opening is spaced from the baffle by a distance of 1cm to 50 cm.
3. The lithium metal powder production apparatus of claim 1, wherein the discharge opening has an outlet diameter of 0.01mm to 5 mm.
4. The lithium metal powder production apparatus according to claim 1, wherein the pressure-resistant container is further provided with a heating means and a heat-insulating means.
5. The lithium metal powder production apparatus according to claim 4, wherein the heating means is provided on the container wall, and the heat insulating means is a heat insulating layer located on the outermost side of the container wall.
6. The lithium metal powder production apparatus of claim 1, wherein the pressure-resistant container further comprises a pressure gauge provided on the wall of the container.
7. The lithium metal powder production apparatus of claim 1, wherein the surface of the baffle is provided with a lithium-phobic protective layer.
8. The lithium metal powder production apparatus according to any one of claims 1 to 7, further comprising a casing forming an enclosed space for accommodating the pressure-resistant container and the baffle.
9. The lithium metal powder production apparatus of claim 8, further comprising a temperature adjustment mechanism for adjusting a temperature of at least one of the baffle plate and the enclosed space.
10. The lithium metal powder production apparatus of claim 9, wherein the temperature adjustment mechanism comprises a coolant line disposed inside the baffle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121156207.XU CN215279880U (en) | 2021-05-27 | 2021-05-27 | Metal lithium powder production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121156207.XU CN215279880U (en) | 2021-05-27 | 2021-05-27 | Metal lithium powder production device |
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| Publication Number | Publication Date |
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| CN215279880U true CN215279880U (en) | 2021-12-24 |
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| CN202121156207.XU Active CN215279880U (en) | 2021-05-27 | 2021-05-27 | Metal lithium powder production device |
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2021
- 2021-05-27 CN CN202121156207.XU patent/CN215279880U/en active Active
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