Reaction device suitable for reducing oxygen-silicon atomic ratio of silicon powder

Abstract

The utility model discloses a reaction device suitable for reducing the oxygen-silicon atomic ratio of silicon powder, the bottom of a reaction tank is provided with an inert gas interface for introducing inert gas, preferably nitrogen, into the reaction tank, and the inert gas moves upwards from the bottom to promote the dissipation of hydrogen, so that the reaction efficiency is improved, and the oxygen-silicon atomic ratio of the silicon powder can be efficiently reduced; a hydrogen concentration detector is arranged at the top of the reaction tank, the hydrogen concentration detector can efficiently detect the concentration of hydrogen in the reaction tank, when the hydrogen concentration is reduced to zero, it can be judged that the reaction is completed, the reaction process can be efficiently and accurately judged through hydrogen concentration detection, and the reaction accuracy is improved; the stirring paddle is uniformly provided with a plurality of stirring holes, the stirring holes are through holes, and the stirring paddle provided with the stirring holes can efficiently puncture hydrogen bubbles in the stirring movement process, so that the dissipation efficiency of hydrogen is improved, and the reaction efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of silicon product preparation, especially to a reaction device suitable for reducing silicon powder oxygen silicon atomic ratio. BACKGROUND

[0002] Lithium ion battery is widely used in various portable electronic devices and electric vehicles due to its large specific energy, high working voltage, long cycle service life, small size, light weight, green environmental protection and other advantages. Currently, the main negative electrode material of commercialized lithium ion battery is graphite, including natural graphite, artificial graphite and the like, but its theoretical specific capacity is only 372mAh / g, which has been difficult to meet the demand of high energy density power supply in the application field of lithium ion battery.

[0003] Nano silicon refers to silicon particles with nanometer level size. Nano silicon powder has the characteristics of high purity, small particle size, uniform distribution, large surface area, high surface activity, low bulk density, non-toxicity and odorlessness. Among non-carbon negative electrode materials, silicon-based material has the highest theoretical lithium intercalation capacity of 4200mAh / g, which is much higher than the theoretical lithium intercalation capacity of other negative electrode materials. In addition, silicon is abundant in reserves (second in the crust element content). Due to the high absorption rate of nano silicon to lithium battery, nano silicon is used in lithium battery to replace nano carbon powder or graphite as negative electrode material of lithium battery. Therefore, nano silicon has become a new generation of negative electrode material of lithium ion battery.

[0004] There is often an oxide layer such as silicon dioxide and silicon monoxide on the surface of nano silicon particles. The existence of silicon dioxide or silicon monoxide surface film seriously affects the theoretical lithium intercalation capacity of nano silicon. Therefore, reducing the oxygen silicon atomic ratio is an effective measure to ensure the theoretical lithium intercalation capacity of nano silicon. UTILITY MODEL CONTENT

[0005] In view of the problems in the related art, the present application discloses a reaction device for reducing the oxygen silicon atomic ratio of silicon powder, which can efficiently reduce the oxygen silicon atomic ratio of silicon powder, improve the purity of nano silicon and improve the reaction efficiency.

[0006] To achieve the above-mentioned purpose, the present application provides the following technical scheme:

[0007] A reaction device suitable for reducing the silicon powder oxygen silicon atomic ratio, comprising a reaction tank, the reaction tank is a sealed tank body, the reaction tank includes a material inlet and a material outlet, the top of the reaction tank is provided with the material inlet, the material inlet is connected with a material supply device, the bottom of the reaction tank is provided with the material outlet, the material outlet is connected with a material discharge device, the top of the reaction tank is also provided with a reaction liquid adding port and an exhaust port, the reaction liquid adding port is connected with a reaction liquid supply device to add reaction liquid, the exhaust port is connected with a gas treatment device to discharge gas, the top of the reaction tank is provided with a stirring power device, the inside of the reaction tank is provided with a stirring device, the stirring power device drives the stirring device to stir, the bottom of the reaction tank is uniformly provided with a plurality of inert gas interfaces, the inert gas interfaces are connected with an inert gas supply device to provide inert gas into the reaction tank.

[0008] As a further scheme of the present application: the top of the reaction tank is provided with a hydrogen concentration detector.

[0009] As a further scheme of the present application: the stirring device includes a stirring shaft, the upper end of the stirring shaft is connected with the stirring power device, the lower end of the stirring shaft is provided with a plurality of stirring paddles, the stirring paddles are long plate-shaped.

[0010] As a further scheme of the present application: two stirring paddles are horizontally symmetrically arranged on the upper part of the stirring shaft, two stirring paddles are horizontally symmetrically arranged on the middle part of the stirring shaft, the stirring paddles on the upper part and the middle part of the stirring shaft are arranged in a cross shape, two upwardly inclined stirring paddles are symmetrically arranged on the lower part of the stirring shaft.

[0011] As a further scheme of the present application: a plurality of stirring holes are uniformly arranged on the stirring paddles, the stirring holes are through holes.

[0012] As a further scheme of the present application: a plurality of stirring needles are uniformly arranged on the stirring paddles, the stirring needles are needle-like rod structures.

[0013] As a further scheme of the present application: the inert gas interface includes an air inlet, the air inlet is connected with the inert gas supply device at the air inlet end, a dispersion cavity is communicated at the air outlet end of the air inlet, a plurality of dispersion holes are arranged on the dispersion cavity, and the dispersion holes uniformly disperse inert gas to the surrounding.

[0014] As a further scheme of the present application: a plurality of supporting legs are arranged on the bottom of the reaction tank, and a weighing sensor is arranged on the bottom of each supporting leg.

[0015] As a further scheme of the present application: a reinforcing rib is fixedly arranged on the top of the reaction tank, and the reinforcing rib is arranged in a cross shape.

[0016] In summary, the beneficial effects of the present application are:

[0017] 1. A reaction device for reducing the atomic ratio of silicon powder to oxygen, the reaction tank is provided with a material inlet, a material outlet, a reaction liquid adding port, an exhaust port, a stirring power device, a stirring device and an inert gas interface, the material enters the reaction tank from the material inlet, an appropriate amount of reaction liquid is added through the reaction liquid adding port, the stirring power device is started to drive the stirring device to rotate to promote the reaction of the material and the reaction liquid to reduce the atomic ratio of oxygen to silicon, the reaction liquid includes an appropriate amount of hydrofluoric acid, the material reacts with the reaction liquid to produce hydrogen gas, the bottom of the reaction tank is provided with an inert gas interface to introduce inert gas into the inside of the reaction tank, preferably nitrogen, the upward movement of the inert gas from the bottom can promote the escape of hydrogen gas, thereby improving the reaction efficiency, the atomic ratio of silicon powder to oxygen can be efficiently reduced, the exhaust port can discharge hydrogen gas, inert gas and reaction gas and is connected with a gas treatment device for gas cleaning treatment, and after the reaction is completed, the material outlet discharges the material to obtain high-purity nano silicon.

[0018] 2. The top of the reaction tank is provided with a hydrogen concentration detector, the hydrogen concentration detector can efficiently detect the hydrogen concentration in the reaction tank, when the hydrogen concentration decreases to zero, it can be determined that the reaction is complete, the reaction process can be accurately determined through the hydrogen concentration detection, and the reaction accuracy is improved.

[0019] 3. A plurality of stirring holes are uniformly arranged on the stirring blade, the stirring holes are through holes, and the stirring blade provided with the stirring holes can efficiently break the hydrogen bubbles during the stirring movement, thereby improving the escape efficiency of hydrogen and the reaction efficiency.

[0020] 4. A plurality of stirring needles are uniformly arranged on the stirring blade, the stirring needles are needle-shaped rod structures, and the stirring blade provided with the stirring needles can efficiently break the hydrogen bubbles during the stirring movement, thereby improving the escape efficiency of hydrogen and the reaction efficiency.

[0021] 5. The inert gas interface comprises a gas inlet, a dispersion cavity and dispersion holes, the dispersion cavity is an arc cavity, the dispersion holes uniformly disperse the inert gas to the surrounding, the uniformity of the inert gas entering the inside of the reaction tank is improved, the uniform pressure of the inert gas can uniformly discharge hydrogen, and the uniformity and reaction efficiency of the silicon powder reaction are improved.

[0022] 6. The bottom of the reaction tank is provided with a plurality of supporting legs, each supporting leg is provided with a weighing sensor at the bottom, the weighing sensor can efficiently and accurately weigh the substances in the reaction tank and the added and escaped substances, thereby improving the reaction accuracy and reaction efficiency.

[0023] 7. The top of the reaction tank is fixedly provided with cross-shaped reinforcing ribs, the reinforcing ribs improve the strength of the reaction tank and improve the reaction safety. BRIEF DESCRIPTION OF DRAWINGS

[0024] The accompanying drawings are included to provide a further understanding of the present application, and are incorporated in and constitute a part of the specification, illustrate embodiments of the present application and are used to explain the present application, but are not intended to limit the present application.

[0025] In the drawings:

[0026] Fig. 1 is a structural schematic diagram of the present application.

[0027] Fig. 2 is a structural schematic diagram of the stirring device of the present application.

[0028] Fig. 3 is a structural schematic diagram of the inert gas interface of the present application.

[0029] Reference signs annotations:

[0030] 1, reaction tank; 2, material inlet; 3, reaction liquid adding port; 4, stirring power device; 5, stirring device; 6, inert gas interface; 7, exhaust port; 8, hydrogen concentration detector; 9, material outlet; 10, supporting leg; 11, weighing sensor; 12, reinforcing rib; 51, stirring shaft; 52, stirring paddle; 53, stirring hole; 54, stirring spike; 61, gas inlet; 62, dispersion cavity; 63, dispersion hole; DETAILED DESCRIPTION

[0031] The exemplary embodiments will be described in detail herein below with reference to the drawings. When the following description refers to the drawings, the same numbers in different drawings represent the same or similar elements unless otherwise indicated. The implementations described in the following exemplary embodiments do not represent all implementations consistent with the present application. Instead, they are merely examples of apparatuses and methods consistent with some aspects of the present embodiments as detailed in the appended claims.

[0032] It should be noted that all directional directions (such as up, down, left, right, front, back, etc.) in the embodiments are only used to explain the relative positional relationship, movement condition, etc. between the components in a certain specific posture (as shown in the drawings), and if the specific posture changes, the directional directions also change accordingly.

[0033] Furthermore, the use of terms such as "first" and "second" in the embodiments is for descriptive purposes only and does not specifically refer to any order or sequence, nor is it intended to limit this application. It is merely to distinguish components or operations described using the same technical terms and should not be construed as indicating or implying their relative importance or implicitly specifying the number of indicated technical features. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the technical solutions of the various embodiments can be combined with each other, but only if they are feasible for those skilled in the art. If a combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed in this application.

[0034] To further understand the content, features, and effects of this application, the following embodiments are provided, and detailed descriptions are given below in conjunction with the accompanying drawings:

[0035] like Figs. 1-3 As shown:

[0036] A reaction apparatus suitable for reducing the oxygen-silicon atomic ratio of silicon powder includes a reaction vessel 1, which is a sealed vessel. The reaction vessel 1 includes a material inlet 2 and a material outlet 9. The material inlet 2 is located at the top of the reaction vessel 1 and is connected to a material supply device, which supplies material to the inside of the reaction vessel 1.

[0037] The bottom of the reaction vessel 1 is provided with a material outlet 9, which is connected to a material discharge device.

[0038] The top of the reaction vessel 1 is also provided with a reaction liquid addition port 3 and an exhaust port 7. The reaction liquid addition port 3 is connected to the reaction liquid supply device to add reaction liquid, which includes hydrofluoric acid.

[0039] The exhaust port 7 is connected to the gas treatment device to discharge gas.

[0040] The top of the reaction vessel 1 is equipped with a stirring power device 4, which includes a motor. The reaction vessel 1 is equipped with a stirring device 5. The stirring power device 4 drives the stirring device 5 to stir, and the stirring of the stirring device 5 enables the materials and the reaction liquid to react fully.

[0041] Four inert gas inlets 6 are evenly provided at the bottom of the reaction vessel 1. The inert gas inlets 6 are connected to the inert gas supply device to supply inert gas into the reaction vessel 1.

[0042] The inert gas interface 6 includes an air inlet 61, the air inlet end of which is connected to an inert gas supply device, and the air outlet end of the air inlet 61 is connected to a dispersion chamber 62. The arc-shaped dispersion chamber 62 is provided with multiple dispersion holes 63, which disperse the inert gas evenly in all directions.

[0043] The reaction tank 1 is provided with a hydrogen concentration detector 8 at the top. Hydrogen is generated by the reaction of hydrofluoric acid and silicon material. The hydrogen concentration detector 8 can efficiently and accurately detect the hydrogen concentration in the reaction tank 1.

[0044] The stirring device 5 includes a stirring shaft 51, the upper end of which is connected to the stirring power device 4, and a plurality of stirring paddles 52 are arranged at the lower end of the stirring shaft 51, which are long plate-shaped.

[0045] Two stirring paddles 52 are horizontally and symmetrically arranged at the upper part of the stirring shaft 51, two stirring paddles 52 are horizontally and symmetrically arranged at the middle part of the stirring shaft 51, and the stirring paddles 52 at the upper and middle parts of the stirring shaft 51 are arranged in a cross shape. Two upwardly inclined stirring paddles 52 are symmetrically arranged at the lower part of the stirring shaft 51.

[0046] Preferably, a plurality of stirring holes 53 are uniformly arranged on the plate of the stirring paddle 52, which are through holes. A plurality of stirring spikes 54 are uniformly arranged around the plate of the stirring paddle 52, which are needle spike rod-shaped structures.

[0047] The reaction tank 1 is provided with three supporting legs 10 at the bottom, and each supporting leg 10 is provided with a weighing sensor 11 at the bottom.

[0048] The reaction tank 1 is fixedly provided with a reinforcing rib 12 at the top, which is arranged in a cross shape.

[0049] In practical application:

[0050] The reaction device is suitable for reducing the silicon atom ratio of silicon powder. The reaction tank 1 is provided with a material inlet 2, a material outlet 9, a reaction liquid adding port 3, an exhaust port 7, a stirring power device 4, a stirring device 5, and an inert gas interface 6.

[0051] The material enters the reaction tank 1 from the material inlet 2, an appropriate amount of reaction liquid is added through the reaction liquid adding port 3, the stirring power device 4 is started to drive the stirring device 5 to rotate to promote the reaction of the material and the reaction liquid to reduce the silicon atom ratio. The reaction liquid includes an appropriate amount of hydrofluoric acid. The material reacts with the reaction liquid to generate hydrogen. The reaction tank 1 is provided with an inert gas interface 6 at the bottom to introduce inert gas into the reaction tank 1. The inert gas is preferably nitrogen. The upward movement of the inert gas from the bottom can promote the escape of hydrogen, thereby improving the reaction efficiency and efficiently reducing the silicon atom ratio of the silicon powder. The exhaust port 7 can exhaust hydrogen, inert gas, and reaction gas and be connected to a gas treatment device for gas cleaning treatment. After the reaction is completed, the material is discharged from the material outlet 9 to obtain high-purity nano silicon.

[0052] The reaction tank 1 is provided with a hydrogen concentration detector 8 at the top. The hydrogen concentration detector 8 can efficiently detect the hydrogen concentration in the reaction tank 1. When the hydrogen concentration decreases to zero, it can be determined that the reaction is complete. The reaction process can be efficiently and accurately determined by detecting the hydrogen concentration, thereby improving the reaction accuracy.

[0053] The stirring blade 52 is uniformly provided with a plurality of stirring holes 53, the stirring holes 53 are through holes, the hydrogen generated by the reaction exists in the form of bubbles, the stirring blade 52 provided with the stirring holes 53 can efficiently break the hydrogen bubbles during the stirring movement, thereby improving the dissipation efficiency of the hydrogen and improving the reaction efficiency.

[0054] The stirring blade 52 is uniformly provided with a plurality of stirring needles 54, the stirring needles 54 are needle-shaped rod structures, the stirring blade 52 provided with the stirring needles 54 can efficiently break the hydrogen bubbles during the stirring movement, thereby improving the dissipation efficiency of the hydrogen and improving the reaction efficiency.

[0055] The inert gas interface 6 includes a gas inlet 61, a dispersion cavity 62 and a dispersion hole 63, the dispersion cavity 62 is an arc cavity, the dispersion hole 63 uniformly disperses the inert gas in all directions, improves the uniformity of the inert gas entering the inside of the reaction tank 1, and the inert gas with uniform pressure can uniformly discharge hydrogen, thereby improving the uniformity of the silicon powder reaction and the reaction efficiency.

[0056] Each support leg 10 is provided with a weighing sensor 11 at the bottom, the weighing sensor 11 can efficiently and accurately weigh the substances in the reaction tank 1 and the added and dissipated substances, thereby improving the reaction accuracy and the reaction efficiency.

[0057] The cross-shaped reinforcing ribs 12 are fixedly arranged at the top of the reaction tank 1, the reinforcing ribs 12 improve the strength of the reaction tank 1 and improve the reaction safety.

[0058] Finally, it should be noted that: the above disclosure is only the preferred embodiment of the present application and is not used to limit the present application, although the present application has been described in detail with reference to the foregoing embodiments, for those skilled in the art, the technical solutions recorded in the foregoing embodiments can be modified, or some technical features can be replaced. Any modification, equivalent replacement, improvement, etc. within the spirit and principles of the present application shall be included in the protection scope of the present application. The scope of the present application is only limited by the appended claims.

Claims

1. A reaction device suitable for reducing the silicon powder oxygen silicon atomic ratio, comprising a reaction tank (1), the reaction tank (1) is a sealed tank body, characterized in that: The reaction tank (1) comprises a material inlet (2) and a material outlet (9), the top of the reaction tank (1) is provided with the material inlet (2), the material inlet (2) is connected with a material supply device, the bottom of the reaction tank (1) is provided with the material outlet (9), the material outlet (9) is connected with a material discharge device, the top of the reaction tank (1) is further provided with a reaction liquid adding port (3) and an exhaust port (7), the reaction liquid adding port (3) is connected with a reaction liquid supply device to add reaction liquid, the exhaust port (7) is connected with a gas treatment device to discharge gas, the top of the reaction tank (1) is provided with a stirring power device (4), the inside of the reaction tank (1) is provided with a stirring device (5), the stirring power device (4) drives the stirring device (5) to stir, the bottom of the reaction tank (1) is uniformly provided with a plurality of inert gas interfaces (6), the inert gas interfaces (6) are connected with an inert gas supply device to provide inert gas into the reaction tank (1).

2. The reaction device for reducing the atomic ratio of silicon powder to silicon oxide according to claim 1, characterized in that: The top of the reaction tank (1) is provided with a hydrogen concentration detector (8).

3. The reaction device for reducing the atomic ratio of silicon to oxygen in silicon powder according to claim 1, characterized in that: The stirring device (5) comprises a stirring shaft (51), the upper end of the stirring shaft (51) is connected with the stirring power device (4), the lower end of the stirring shaft (51) is provided with a plurality of stirring paddles (52), and the stirring paddles (52) are long plate-shaped.

4. The reaction device for reducing the atomic ratio of silicon to oxygen of silicon powder according to claim 3, characterized by: Two stirring paddles (52) are horizontally and symmetrically arranged on the upper part of the stirring shaft (51), two stirring paddles (52) are horizontally and symmetrically arranged on the middle part of the stirring shaft (51), the stirring paddles (52) on the upper part and the middle part of the stirring shaft (51) are arranged in a cross shape, and two upwardly inclined stirring paddles (52) are symmetrically arranged on the lower part of the stirring shaft (51).

5. The reaction apparatus for reducing the atomic ratio of silicon to oxygen in silicon powder according to claim 3, characterized by: A plurality of stirring holes (53) are uniformly arranged on the stirring paddles (52), and the stirring holes (53) are through holes.

6. The reaction apparatus for reducing the atomic ratio of silicon to oxygen in silicon powder according to claim 3, characterized by: A plurality of stirring needles (54) are uniformly arranged on the stirring paddles (52), and the stirring needles (54) are needle-stick rod-shaped structures.

7. The reaction apparatus for reducing the atomic ratio of silicon to oxygen in silicon powder according to claim 1, characterized by: The inert gas interface (6) comprises an air inlet (61), the air inlet (61) is connected with the inert gas supply device at the air inlet end, a dispersion cavity (62) is arranged at the air outlet end of the air inlet (61) in communication, a plurality of dispersion holes (63) are arranged on the dispersion cavity (62), and the inert gas is uniformly dispersed in all directions through the dispersion holes (63).

8. The reaction apparatus for reducing the atomic ratio of silicon to oxygen in silicon powder according to claim 1, characterized by: The bottom of the reaction tank (1) is provided with a plurality of supporting legs (10), and the bottom of each supporting leg (10) is provided with a weighing sensor (11).

9. The reaction apparatus for reducing the atomic ratio of silicon to oxygen of silicon powder according to claim 1, characterized by: The top of the reaction tank (1) is fixedly provided with a reinforcing rib (12), and the reinforcing rib (12) is arranged in a cross shape.

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