Gallium impurity removal device

Abstract

The utility model discloses an impurity removal device for metal gallium. The technical problem that in the prior art, the energy utilization rate is not high is solved. The metal gallium impurity removal device comprises a heating tank used for containing a heating medium, the heating tank is provided with a water inlet and a water outlet, the water inlet and the water outlet are located in the two opposite sides of the heating tank, and the water inlet and the water outlet are both communicated with a cooling circulating water pipeline of an aluminum oxide production line; the pickling tank is located in the heating tank and provided with a material inlet and a material outlet, and the material inlet and the material outlet are both located outside the heating tank; the stirrer is positioned in the pickling tank; and the heater is positioned in the heating tank and is positioned outside the pickling tank. According to the device, heat energy recycling is achieved, the energy utilization rate is increased, the temperature uniformity of cooling circulating water is guaranteed, the temperature uniformity of acid liquor and metal gallium in the acid liquor tank is improved, and the purification effect is stabilized.

Description

Technical Field

[0001] The present application belongs to the technical field of metal gallium impurity removal, and specifically relates to a metal gallium impurity removal device. Background Art

[0002] Gallium metal with a purity of 6N or above is called high-purity gallium. It is an important raw material for preparing various gallium compounds (gallium arsenide, gallium nitride, gallium oxide). With the continuous advancement of my country's electronics and communications industry technology, the role of high-purity gallium in the development of my country's semiconductor industry is becoming increasingly prominent.

[0003] High-purity gallium is produced by purifying 4N gallium metal as raw material, and the quality of 4N gallium metal raw material directly affects the purification of high-purity gallium. However, the 4N gallium metal extracted from alumina mother liquor through resin adsorption and electrolytic refining process has high content of impurity elements such as zinc and iron, and there are surface oxidation phenomena, which have an adverse effect on the purification of high-purity gallium. Therefore, before the purification of gallium metal, the 4N gallium metal raw material needs to be acid-washed and impurity-removed.

[0004] Most of the existing pickling and impurity removal devices use heating wires as heating structures and utilize additional electrical energy for heating, resulting in low energy utilization. Utility Model Content

[0005] In order to solve the technical problem of low energy utilization rate of current pickling and impurity removal devices, the present application provides a pickling and impurity removal device.

[0006] The present application provides a metal gallium impurity removal device, comprising:

[0007] A heating tank, used to contain a heating medium, the heating tank is provided with a water inlet and a water outlet, the water inlet and the water outlet are located on opposite sides of the heating tank, and the water inlet and the water outlet are both connected to a cooling circulating water pipeline of the alumina production line;

[0008] A pickling tank is located inside the heating tank and is provided with a material inlet and a material outlet, wherein the material inlet and the material outlet are both located outside the heating tank;

[0009] an agitator, located in the pickling tank;

[0010] The heater is located in the heating tank and outside the pickling tank.

[0011] In some embodiments, the pickling tank includes a drain pipe and an on-off valve installed on the drain pipe, the drain pipe is connected to the bottom of the pickling tank, the drain pipe extends out of the heating tank, and the mouth of the drain pipe forms the material outlet.

[0012] In some embodiments, the heating tank is provided with an avoidance groove with a notch facing downward, the drain pipe extends into the avoidance groove, and the on-off valve is located in the avoidance groove; the on-off valve is a flow regulating valve.

[0013] In some embodiments, a protrusion is provided inside the heating tank, and the protrusion forms the avoidance groove outside the heating tank. The vertical wall of the protrusion has a smooth transition with the tank body and the protruding top of the heating tank.

[0014] In some embodiments, the radial dimension of the bottom of the pickling tank decreases from top to bottom, and the lowest point of the pickling tank is close to the protrusion.

[0015] In some embodiments, the pickling tank further includes an auxiliary heater, and the auxiliary heater is coated on the outer wall of the drain pipe.

[0016] In some embodiments, the height of the water inlet is lower than the height of the water outlet.

[0017] In some embodiments, a temperature sensor and a controller are further included. The temperature sensor is used to detect the temperature of the cooling circulating water in the heating tank, and the controller is electrically connected to the temperature sensor and the heater.

[0018] In some embodiments, a driving member and a telescopic member are further included, wherein the driving member has a rotatable output end connected to the agitator, and the telescopic member can reciprocate and telescope in a vertical direction, and the telescopic end of the telescopic member is connected to the driving member.

[0019] In some embodiments, a dust cover is further included, the pickling tank has an opening, and the dust cover can be opened and closed to close the opening;

[0020] It also includes a bracket and a base, the heating tube is installed on the bracket, and the telescopic member is installed on the base;

[0021] The bracket is a stainless steel bracket, the base is a stainless steel base, or,

[0022] The bracket and the base are both covered with an anti-corrosion layer.

[0023] The gallium metal impurity removal device provided according to the embodiment of the present application includes a heating tank, a pickling tank, a stirrer and a heater, wherein the heating tank is used to accommodate a heating medium, and the heating tank is provided with a water inlet and a water outlet, and the water inlet and the water outlet are located on opposite sides of the heating tube, so that the heating medium forms convection in the heating tank, which is convenient for heat exchange of the pickling tank, and the water inlet and the water outlet are both connected to the cooling circulating water pipeline of the alumina production line, so that the gallium metal material extracted from the alumina mother liquor in the alumina production line can be used as a raw material for gallium metal purification, and the heat in the cooling circulating water of the alumina production line, such as the evaporation workshop, can be used to heat the pickling tank, so that the gallium metal remains in a liquid state, so as to achieve Energy is recycled; the pickling tank is located in the heating tank and is provided with a material inlet and a material outlet. The material inlet can be used to add metal gallium and acid liquid, and the material outlet can be used to discharge the purified metal gallium and acid liquid containing impurities. The material inlet and the material outlet are both located outside the heating tank to facilitate the feeding and discharging operations; the agitator is located in the pickling tank to stir the metal gallium and acid liquid in the pickling tank to improve the purification efficiency; the cooling circulating water temperature of the alumina production line is sometimes high and sometimes low, and the temperature is unstable. The heater is located in the heating tank and outside the pickling tank. The heating can be started when the cooling circulating water temperature is low to improve the temperature uniformity of the cooling circulating water, thereby ensuring the purification effect.

[0024] Compared with the prior art, the present application adopts the cooling circulating water of the alumina production line as the main heating source, and adopts a heater to heat the cooling circulating water when the temperature is not high enough, which not only realizes the recovery and utilization of heat energy and improves the energy utilization rate, but also ensures the temperature uniformity of the cooling circulating water, improves the temperature uniformity of the acid in the acid tank and the metal gallium, and stabilizes the purification effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 A schematic structural diagram of a metal gallium impurity removal device in one or more embodiments of the present application is shown.

[0026] Description of reference numerals:

[0027] 10-heating tank, 11-water inlet, 12-water outlet, 13-avoidance groove, 20-pickling tank, 21-material inlet, 22-material outlet, 23-drain pipe, 24-on and off valve, 25-auxiliary heater, 26-tank body, 30-agitator, 40-heater, 50-driving part, 60-telescopic part, 70-bracket, 80-base, 90-dust cover. DETAILED DESCRIPTION

[0028] In order to make the technical personnel in the technical field to which the present application belongs to understand the present application more clearly, the technical scheme in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present application.

[0029] Raw material gallium

[0030] The present application provides a metal gallium impurity removal device, which not only realizes the recovery and utilization of heat energy and improves the energy utilization rate, but also ensures the temperature uniformity of the cooling circulating water, improves the temperature uniformity of the acid in the acid tank and the metal gallium, and stabilizes the purification effect.

[0031] See also Figure 1 The gallium metal impurity removal device provided in the present application includes a heating tank 10, a pickling tank 20, an agitator 30 and a heater 40, wherein the heating tank 10 is used to accommodate a heating medium, and the heating tank 10 is provided with a water inlet 11 and a water outlet 12, and the water inlet 11 and the water outlet 12 are located on opposite sides of the heating tube, so that the heating medium forms convection in the heating tank 10, which is convenient for heat exchange with the pickling tank 20, and the water inlet 11 and the water outlet 12 are both connected to the cooling circulating water pipeline of the alumina production line, so that the high-temperature cooling water in the cooling circulating water pipeline enters from the water inlet 11, and is then discharged from the water outlet 12 to the cooling circulating water pipeline to participate in the cooling circulation of the alumina production line. Therefore, the gallium-containing material extracted from the alumina mother liquor in the alumina production line can be used as a raw material for gallium metal purification, and the heat in the cooling circulating water of the alumina production line, such as the evaporation workshop, can be used to heat the pickling tank 20, so that the gallium metal remains in a liquid state, so as to achieve Energy is recycled; the pickling tank 20 is located in the heating tank 10, and is provided with a material inlet 21 and a material outlet 22. The material inlet 21 can be used to add metal gallium and acid solution. The acid solution can react chemically with zinc impurities and iron impurities in the metal gallium to form salt and enter the acid solution. The metal gallium liquid and the acid solution will be separated into layers, with the metal gallium liquid having a high density at the bottom and the acid solution at the top. The material outlet 22 can be used to discharge the purified metal gallium and the acid solution containing impurities. The material inlet 21 and the material outlet 22 are both located outside the heating tank 10 to facilitate the feeding and discharging operations; the agitator 30 is located in the pickling tank 20 to stir the metal gallium and the acid solution in the pickling tank 20 to improve the purification efficiency; the heater 40, such as a heating rod, is located in the heating tank 10 and outside the pickling tank 20 to start heating when the temperature of the cooling circulating water is low, for example, heating is started by passing alternating current, and cooperates with the cooling circulating water to improve the temperature uniformity of the cooling circulating water, thereby ensuring the purification effect.

[0032] See also Figure 1 In some embodiments, the height of the water inlet 11 is lower than the height of the water outlet 12, that is, the cooling circulating water enters from the bottom and exits from the top, optimizing the flow field of the heating medium in the heating tank 10 and improving the heat exchange effect between the cooling circulating water and the pickling tank 20. In other embodiments, the height of the water inlet 11 is higher than the height of the water outlet 12, or the height of the water inlet 11 is the same as the height of the water outlet 12, which can also achieve the inlet and outlet of the cooling circulating water and the heat exchange between the cooling circulating water and the pickling tank 20.

[0033] In some embodiments, the number of water inlets 11 and water outlets 12 can be multiple, and a multi-inlet and multi-outlet method can be adopted to increase the temperature at the outlet of the cooling circulating water and improve the temperature uniformity of the metal gallium liquid in the pickling tank 20.

[0034] The melting point of metallic gallium is 29.76°C and its density is 5.904 g / cm 3 , density is higher than that of the acid solution, so the gallium metal is at the bottom and the acid solution is at the top, see Figure 1 In some embodiments, the pickling tank 20 includes a tank body 26 and a drain pipe 23. The bottom of the tank body 26 is connected to the drain pipe 23. The drain pipe 23 extends out of the heating tank 10. The mouth of the drain pipe 23 forms a material outlet 22. A drain port is provided at the bottom, so that the gallium metal can be discharged first and then the acid liquid, and there is no residue after the discharge. In other embodiments, the side of the pickling tank 20 is connected to the drain pipe 23, which can also realize the discharge function of the gallium metal and the acid liquid. In some other embodiments, the drain port of the pickling tank 20 is connected to the siphon structure to realize the demand for discharging the gallium metal.

[0035] In order to reduce the volume of the metal gallium in the discharge pipe 23 which is difficult to be stirred by the stirrer 30 and has poor fluidity, and ensure the purification effect of the metal gallium, please refer to Figure 1 The heating tank 10 is provided with an avoidance groove 13 with a notch facing downward, and a drain pipe 23 extends into the avoidance groove 13. The pickling tank 20 includes an on-off valve 24 installed on the drain pipe 23, which is used to realize the conduction and cutoff of the drain pipe 23. When the drain pipe 23 is conducted, the metal gallium and the acid solution can be discharged from the drain pipe 23 in sequence. When the drain pipe 23 is cut off, the metal gallium and the acid solution are kept in the acid tank for impurity removal and purification.

[0036] In some embodiments, the on-off valve 24 may be a flow regulating valve, the opening of which can be adjusted from zero to the maximum. When the opening of the flow regulating valve is zero, the drain pipe 23 is cut off. When the opening of the flow regulating valve is greater than zero, the drain pipe 23 is turned on. When the drain pipe 23 is turned on, the opening of the flow regulating valve is adjustable to achieve flow regulation of the metal gallium liquid. When drainage is required, the flow regulating valve is first opened to a very small opening, so that the metal gallium liquid gradually flows out, and then slowly adjusted to a large opening to increase the discharge rate of the metal gallium liquid.

[0037] See also Figure 1 In one embodiment, the on-off valve 24 is located in the avoidance groove 13, which can reduce the volume of the metal gallium in the drain pipe 23, thereby reducing the proportion of the metal gallium dead zone and improving the purification purity of the metal gallium. In another embodiment, the heating tank 10 is not provided with the avoidance groove 13, and the on-off valve 24 is located outside the heating tank 10, which can also achieve the purification of the metal gallium and the conduction and cutoff of the drain pipe 23.

[0038] See also Figure 1 In one embodiment, a protrusion is provided inside the heating tank 10, and the protrusion forms an avoidance groove 13 outside the heating tank 10, and the vertical wall of the protrusion smoothly transitions with the tank body 26 of the heating tank 10, and the vertical wall smoothly transitions with the convex top, so that the inner wall of the heating tank 10 is arc-shaped, so as to reduce the dead zone ratio of the cooling circulating water in the heating tank 10, improve the flow field of the cooling circulating water, and improve the heat exchange effect between the cooling circulating water and the acid tank. In some embodiments, the shape of the protrusion can be a hemispherical protrusion, a cylindrical protrusion, a conical protrusion, etc. In another embodiment, the bottom wall inside the heating tank 10 is a curved surface or a flat surface, which can also reduce the dead zone ratio of the cooling circulating water in the heating tank 10.

[0039] Please continue reading Figure 1 In some embodiments, the radial dimension of the bottom of the pickling tank 20 decreases from top to bottom, forming a quasi-truncated cone structure, which can further reduce the proportion of the metal gallium dead zone in the pickling tank 20 and improve the stirring effect and purification effect; and the quasi-truncated cone bottom structure also increases the heat exchange area between the cooling circulating water and the pickling tank 20, thereby improving the heat exchange effect. The lowest point of the bottom of the pickling tank 20 is close to the protrusion, which can further shorten the metal gallium liquid above the opening and closing valve 24 in the drain pipe 23, thereby improving the stirring effect and purification effect of the metal gallium.

[0040] Please continue reading Figure 1 In some embodiments, the pickling tank 20 further includes an auxiliary heater 25 coated on the outer wall of the drain pipe 23 to heat the metal gallium liquid during the drainage process to prevent the metal gallium from freezing and crystallizing due to too low a temperature and blocking the drain pipe 23, thereby improving the drainage patency; the auxiliary heating device may be a heating wire, which may be spirally coated on the outside of the drain pipe 23, or may be arranged in a serpentine shape on the outer wall of the drain pipe 23. In other embodiments, the temperature of the cooling circulating water may be increased by the heater 40, that is, the superheat of the metal gallium may be increased, so that the metal gallium liquid is always above the melting point during the process of being discharged from the drain pipe 23.

[0041] In some embodiments, the metal gallium impurity removal device further includes a temperature sensor and a controller, wherein the temperature sensor is used to detect the temperature of the cooling circulating water in the heating tank 10, and the controller is electrically connected to the temperature sensor and the heater 40. The temperature sensor sends the detected cooling circulating water temperature to the controller, and the controller receives the temperature emitted by the temperature sensor and compares the temperature with the set value. When the temperature is lower than the set value, the controller controls the heater 40 to turn on, and the heater 40 heats the cooling circulating water.

[0042] For the stirrer 30, a stirring paddle can be selected, and its material can be selected from polytetrafluoroethylene, which can withstand a heating temperature of 1500°C and is also resistant to acid corrosion. The stirring paddle can be cleaned with strong acid and high-purity water. Figure 1 In some embodiments, the gallium metal impurity removal device includes a driving member 50 and a telescopic member 60. The driving member 50 may be a driving motor. The driving member 50 has a rotatable output end, which is connected to the agitator 30 to drive the agitator 30 to rotate, stir the gallium metal and the acid in the acid tank, and improve the purification effect. The telescopic member 60 may be an electric cylinder or a hydraulic cylinder. The telescopic member 60 may be reciprocated in the vertical direction. The telescopic end of the telescopic member 60 is connected to the driving member 50 to adjust the height of the driving member 50, thereby driving the agitator 30 to adjust the height to adapt to different liquid levels of acid and gallium metal liquid. In other embodiments, the gallium metal impurity removal device includes a lead screw slider mechanism, and the height adjustment of the driving member 50 can also be achieved through the lead screw slider structure.

[0043] The telescopic end of the telescopic member 60 can be connected to the housing of the driving member 50 through a connecting rod. The telescopic member 60 and the driving member 50 are both electrically connected to a controller. The controller can adjust the telescopic length of the telescopic member 60, thereby adjusting the suspension height of the stirrer 30 to meet the stirring height requirements of different liquid levels. The controller can control the rotation speed of the driving member 50, thereby controlling the rotation speed of the stirrer 30 to meet different stirring requirements.

[0044] See also Figure 1 In some embodiments, the gallium metal impurity removal device further includes a dust cover 90. The pickling tank 20 has an opening. The dust cover 90 can be opened and closed to close the opening to prevent foreign matter and dust from falling onto the surface of the acid solution, reduce environmental and personnel pollution of the material, and prevent external impurities from affecting the pickling effect during the gallium metal pickling process; it can also prevent the acid solution from volatilizing and improve the utilization rate of the acid solution. The dust cover 90 is provided with a through hole, and the stirring shaft of the stirrer 30 is passed through the through hole.

[0045] Please continue reading Figure 1In some embodiments, the metal gallium impurity removal device further includes a bracket 70 and a base 80, the heating tank 10 is installed on the bracket 70, the telescopic member 60 is installed on the base 80, and the bracket 70 and the base 80 are both made of stainless steel, or the surfaces of the bracket 70 and the base 80 are covered with an anti-corrosion layer, so that they still have good corrosion resistance when acid splashes, thereby extending the service life of the metal gallium impurity removal device.

[0046] In some embodiments, the metal gallium impurity removal device further includes a display screen, which can display the temperature of the cooling circulating water, making it more intuitive.

[0047] The metal gallium impurity removal device provided in the present application adopts the cooling circulating water of the alumina production line as the main heating source, and adopts the heater 40 for heating when the temperature of the cooling circulating water is not high enough, which not only realizes the recovery and utilization of heat energy and improves the energy utilization rate, but also ensures the temperature uniformity of the cooling circulating water, improves the temperature uniformity of the acid in the acid tank and the metal gallium, and stabilizes the purification effect; the metal gallium impurity removal device can carry out acid washing and impurity removal on the raw material 4N gallium after electrolysis, reduce the impurity concentration of the gallium raw material, and ensure the quality of the subsequent high-purity gallium product.

[0048] In the present application, unless otherwise clearly specified and limited, a first feature being "above" or "below" a second feature may include that the first and second features are in direct contact, or may include that the first and second features are not in direct contact but are in contact through another feature between them. Moreover, a first feature being "above", "above" and "above" a second feature includes that the first feature is directly above and obliquely above the second feature, or simply indicates that the first feature is higher in level than the second feature. A first feature being "below", "below" and "below" a second feature includes that the first feature is directly below and obliquely below the second feature, or simply indicates that the first feature is lower in level than the second feature.

[0049] In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise" and "counterclockwise" indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present application.

[0050] In this application, unless otherwise clearly specified and limited, the terms "connection", "fixation", etc. should be understood in a broad sense. For example, "fixation" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, it can be the internal connection of two elements or the interaction relationship between two elements. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0051] In addition, the descriptions of "first", "second", etc. in this application are only for descriptive purposes and cannot be understood as indicating or implying their relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" or "second" may explicitly or implicitly include one or more features. In the description of this application, the meaning of "plurality" is two or more, unless otherwise clearly and specifically defined.

[0052] Although the embodiments of the present application have been shown and described, those skilled in the art will appreciate that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present application, and that the scope of the present application is defined by the claims and their equivalents.

Claims

1. A metal gallium impurity removal device, characterized in that: include: A heating tank, used to contain a heating medium, the heating tank is provided with a water inlet and a water outlet, the water inlet and the water outlet are located on opposite sides of the heating tank, and the water inlet and the water outlet are both connected to a cooling circulating water pipeline of the alumina production line; A pickling tank is located inside the heating tank and is provided with a material inlet and a material outlet, wherein the material inlet and the material outlet are both located outside the heating tank; an agitator, located in the pickling tank; The heater is located in the heating tank and outside the pickling tank.

2. The metal gallium impurity removal device according to claim 1, characterized in that: The pickling tank includes a drain pipe and an on-off valve installed on the drain pipe. The drain pipe is connected to the bottom of the pickling tank and extends out of the heating tank. The pipe mouth of the drain pipe forms the material outlet.

3. The metal gallium impurity removal device according to claim 2, characterized in that: The heating tank is provided with an escape groove with a notch facing downwards, the drain pipe extends into the escape groove, and the on-off valve is located in the escape groove; the on-off valve is a flow regulating valve.

4. The metal gallium impurity removal device according to claim 3, characterized in that: A protrusion is provided inside the heating tank, and the protrusion forms the avoidance groove outside the heating tank. The vertical wall of the protrusion has a smooth transition with the tank body and the convex top of the heating tank.

5. The metal gallium impurity removal device according to claim 4, characterized in that: The radial dimension of the bottom of the pickling tank decreases in a direction from top to bottom, and the lowest point of the pickling tank is close to the protrusion.

6. The metal gallium impurity removal device according to any one of claims 2 to 5, characterized in that: The pickling tank further includes an auxiliary heater, and the auxiliary heater is coated on the outer wall of the drain pipe.

7. The metal gallium impurity removal device according to any one of claims 1 to 5, characterized in that: The height of the water inlet is lower than that of the water outlet.

8. The metal gallium impurity removal device according to any one of claims 1 to 5, characterized in that: It also includes a temperature sensor and a controller. The temperature sensor is used to detect the temperature of the cooling circulating water in the heating tank. The controller is electrically connected to the temperature sensor and the heater.

9. The metal gallium impurity removal device according to any one of claims 1 to 5, characterized in that: It also includes a driving member and a telescopic member. The driving member has a rotatable output end connected to the agitator. The telescopic member can reciprocate and telescope in a vertical direction. The telescopic end of the telescopic member is connected to the driving member.

10. The metal gallium impurity removal device according to claim 9, characterized in that: It also includes a dust cover, the pickling tank has an opening, and the dust cover can be opened and closed to close the opening; It also includes a bracket and a base, the heating tube is installed on the bracket, and the telescopic member is installed on the base; The bracket is a stainless steel bracket, the base is a stainless steel base, or, The bracket and the base are both covered with an anti-corrosion layer.

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