LED gallium and indium recycling device
By designing the LED gallium indium recycling device, using multiple reactors and processing systems to extract gallium and indium elements in MOCVD waste in stages, the problem of low resource recycling efficiency in the prior art is solved, and efficient gallium and indium element recycling and energy conservation and emission reduction are achieved.
Patent Information
- Application Number
- CN202510191178.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-20
- Publication Date
- 2025-05-02
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The prior art is difficult to effectively recycle and utilize gallium and indium elements in MOCVD waste generated during LED production, resulting in low resource recycling efficiency and poor selectivity.
An LED gallium indium recycling device is designed, which includes multiple reactors, filters, stirring systems, temperature control systems and liquid treatment systems. By extracting and processing MOCVD waste powder in segments, the effective recycling of gallium and indium elements is achieved.
The device can effectively reduce solid waste emissions, improve the recovery rate of gallium and indium elements, save costs and reduce energy consumption.
Smart Images
Figure CN119909620A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of recycling gallium-indium-containing waste materials, and in particular to an LED gallium-indium recycling device. Background Art
[0002] LED is widely used in many fields due to its advantages of high efficiency, low energy consumption, long life, safety, no mercury, fast response, wide application and flexible control. With the popularity of LED and its growing market penetration, the demand for rare and precious metals such as indium, gallium and copper has increased dramatically. In addition, a large amount of solid waste is generated during the production and consumption process.
[0003] At present, the phase composition of MOCVD waste in solid waste is relatively simple, mainly composed of GaN and indium single phases, as shown in Table 1. However, GaN is a difficult to dissolve and melt material, which makes the recycling of MOCVD waste resources more difficult, with low resource recycling efficiency and poor selectivity. Therefore, LED gallium indium recycling equipment is urgently needed to solve the above problems.
[0004] Table 1 Elemental composition of MOCVD waste Summary of the invention The purpose of the present invention is to provide an LED gallium-indium recycling device to solve the problems raised in the above background technology.
[0005] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: an LED gallium indium recycling device comprises a first reactor, the first reactor, the upper end of the first reactor is connected with a pipeline, the other side of the pipeline is connected with a condenser, the other side of the condenser is connected to a Monteggia washing bottle through a pipeline, one side of the first reactor is connected to an atmosphere box-type protection electric furnace, a filter is connected to the bottom of the first reactor, a jacket is provided on the outer layer of the first reactor, a first circulating oil bath is provided at the bottom of the first reactor, the jacket is connected to the first circulating oil bath, a reduction motor is provided above the first reactor, a stirring shaft is installed at the output end of the reduction motor, the stirring shaft is connected to the first reactor, an alkali solution storage tank is provided on the right side of the first reactor, a clean water tank is provided on the right side of the alkali solution storage tank, the alkali solution storage tank and the clean water tank are both connected to the first reactor with a pipeline, and a temperature sensor and a sensor are also provided in the first reactor.
[0006] As a preferred technical solution of the present invention, an alkali solution washing tank is provided on the right side of the filter, an alkali solution buffer tank is provided on the side of the alkali solution washing tank away from the filter, a second reactor is provided on the right side of the alkali solution buffer tank, the bottom end of the second reactor is respectively connected to a second circulating oil bath and a filter through pipelines, and the upper end of the second reactor is connected to an acid storage tank through a pipeline.
[0007] As a preferred technical solution of the present invention, the right side of the second reactor is connected to an acid washing tank and an acid buffer tank through pipelines, and multiple discharge valves are provided on the pipelines between the acid washing tank and the acid buffer tank and the second reactor for regulation.
[0008] As a preferred technical solution of the present invention, an air compressor is connected to the pipeline between the first reactor and the second reactor, and a pressure regulating valve for regulating the air compressor is provided on the pipeline between the air compressor and one side.
[0009] As a preferred technical solution of the present invention, an air outlet is provided on the atmosphere box-type protection electric furnace, and the air outlet is connected to the pipeline. A supporting leg is fixedly installed at the bottom of the atmosphere box-type protection electric furnace for supporting effect. A rotor flowmeter is provided on one side of the atmosphere box-type protection electric furnace. A control panel for controlling effect is installed in the atmosphere box-type protection electric furnace.
[0010] As a preferred technical solution of the present invention, a solenoid valve is installed between the first reactor and the clean water tank, and a peristaltic pump is provided between the first reactor and the alkali solution storage tank, wherein a feeding valve and a drain valve are respectively installed on the alkali solution storage tank, and the feeding valve and the drain valve are symmetrically arranged on both sides of the alkali solution storage tank.
[0011] As a preferred technical solution of the present invention, a stirring blade is fixedly installed at the bottom end of the stirring shaft, and an interface is installed at the bottom end of the first reactor, and the interface is connected to the pipeline.
[0012] As a preferred technical solution of the present invention, the alkali solution storage tank, the first reaction kettle, the alkali solution washing tank and the alkali solution buffer tank are all made of stainless steel 316L.
[0013] As a preferred technical solution of the present invention, the second reactor is made of high borosilicate glass material for storing liquid and reacting, and the acid washing tank and the acid buffer tank are both made of corrosion-resistant PE material.
[0014] As a preferred technical solution of the present invention, the working chamber volume of the atmosphere box-type protection electric furnace is 8L, the maximum temperature is 1200°C, and an air outlet is provided on the front, wherein the exhaust gas is connected to the Mengshi washing bottle through a pipeline for exhaust gas adsorption treatment.
[0015] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention is an LED gallium-indium recycling device. The LED gallium-indium recycling device provided by the present invention can reduce the discharge of solid waste by effectively extracting gallium-indium elements from MOCVD waste powder in the LED production process in segments. At the same time, it can also effectively recycle metal elements, which is beneficial to saving costs and reducing energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.
[0017] Figure 1 is a schematic structural diagram of an LED gallium-indium recycling device according to an embodiment of the present invention; Figure 2 2 is a schematic structural diagram of an atmosphere box-type protection electric furnace for an LED gallium-indium recycling device according to an embodiment of the present invention; Figure 3 1 is a schematic diagram of the structure of the first reactor of the LED gallium-indium recycling device according to an embodiment of the present invention.
[0018] Reference numerals: 1. First reactor; 2. Condenser; 3. Pipeline; 4. Montex washing bottle; 5. Peristaltic pump; 6. Alkali storage tank; 7. Feeding valve; 8. Vent valve; 9. Solenoid valve; 10. Clean water tank; 11. Filter; 12. First circulation oil bath; 13. Alkali washing tank; 14. Alkali buffer tank; 15. Pressure regulating valve; 16. Air compressor; 17. Second circulation oil bath; 18. Second reactor; 19. Acid storage tank; 20. Vent valve; 21. Acid washing tank; 22. Acid buffer tank; 23. Atmosphere box protection electric furnace; 24. Air outlet; 25. Rotor flowmeter; 26. Control panel; 27. Support leg; 28. Reducer motor; 29. Stirring shaft; 30. Temperature sensor; 31. Sensor; 32. Jacket; 33. Stirring fan blade; 34. Interface. DETAILED DESCRIPTION
[0019] Below, the invention is further described in conjunction with the accompanying drawings and specific embodiments: Example 1 refer to Figure 1 to Figure 2Embodiment 1 is described, comprising a first reactor 1, a first reactor 1, an upper end of the first reactor 1 is connected to a pipeline 3, the other side of the pipeline 3 is connected to a condenser 2, the other side of the condenser 2 is connected to a Monteggia bottle washing bottle 4 through a pipeline, one side of the first reactor 1 is connected to an atmosphere box-type protection electric furnace 23, firstly, the material is placed in the atmosphere box-type protection electric furnace 23 and fired into powder, and the fired powder is transported to the first reactor 1 through the pipeline powder, without manual feeding, a filter 11 is connected to the bottom of the first reactor 1, and the outer layer of the first reactor 1 is provided with A jacket 32 is provided at the bottom of the first reactor 1 with a first circulating oil bath 12, the jacket 32 is connected to the first circulating oil bath 12, a reduction motor 28 is provided above the first reactor 1, a stirring shaft 29 is installed at the output end of the reduction motor 28, the stirring shaft 29 is connected to the first reactor 1, an alkali liquid storage tank 6 is provided on the right side of the first reactor 1, a clean water tank 10 is provided on the right side of the alkali liquid storage tank 6, the alkali liquid storage tank 6 and the clean water tank 10 are connected to the first reactor 1 with a pipeline 3, and a temperature sensor 30 and a sensor 31 are also provided in the first reactor 1, and the atmosphere chamber The atmosphere box type protection electric furnace 23 is provided with an air outlet 24, which is connected to the pipeline 3. A support leg 27 is fixedly installed at the bottom of the atmosphere box type protection electric furnace 23 for supporting the electric furnace. A rotor flow meter 25 is provided on one side of the atmosphere box type protection electric furnace 23. A control panel 26 for controlling the electric furnace 23 is installed inside the atmosphere box type protection electric furnace 23. A solenoid valve 9 is installed between the first reaction kettle 1 and the clean water tank 10. A peristaltic pump 5 is provided between the first reaction kettle 1 and the alkali solution storage tank 6. A feeding valve 7 and a venting valve 8 are respectively installed on the alkali solution storage tank 6. , and the feeding valve 7 and the venting valve 8 are symmetrically arranged on both sides of the alkali liquid storage tank 6, the stirring shaft 29 is fixedly installed with a stirring blade 33 at the bottom end, the first reactor 1 is installed with an interface 34 at the bottom end, and the interface 34 is connected to the pipeline 3, the alkali liquid storage tank 6, the first reactor 1, the alkali liquid washing tank 13 and the alkali liquid buffer tank 14 are all made of stainless steel 316L, the working room volume of the atmosphere box protection electric furnace 23 is 8L, the maximum temperature is 1200℃, and the front is provided with an outlet 24, wherein the exhaust gas is connected to the Mengshi washing bottle 4 through the pipeline 3 for exhaust gas adsorption treatment; In this embodiment, the material is first pretreated using an atmosphere box-type protective electric furnace 23. The roasting pretreatment is carried out in an air atmosphere. The atmosphere box-type protective electric furnace 23 is kept at a constant temperature of 1050°C for 3 hours to oxidize the metal indium and GaN to obtain Ga2O3 and In2O3, thereby improving the leaching performance of GaN and indium. The roasted material is added to the first reactor 1 through the solid feed port. The alkali solution in the alkali solution storage tank 6 is added to the reactor by controlling the flow rate of the peristaltic pump 5. The first circulating oil bath 12 is turned on, the heating temperature is set, and the jacket 32 on the first reactor 1 is heated. The non-condensable steam in the first reactor 1 can be connected to the Monte Carlo washing bottle 4 through the outlet of the condenser 2 to absorb the tail gas. After the reaction is completed, gallium selectively enters the solution, and the leaching rate of indium is lower than 1. %, to achieve preliminary separation of gallium and indium, complete filtration and washing, obtain crude indium slag product, naturally cool to below 50°C, manually open the bottom valve of the bottom tank of the first reactor 1, and the feed liquid enters the filter 11; turn on the air compressor 16, close the vent valve 8 of the filter 11, adjust the pressure regulating valve 15, open the valve for solid-liquid separation, the solid is trapped in the filter 11, open the quick release at the bottom of the filter to collect the solid material, and the liquid enters the alkali solution buffer tank 14; water washing: open the solenoid valve 9, and the water in the alkali solution washing tank 13 is added to the kettle through the peristaltic pump 5, and the jacket 32 is used for heating. The residual heat is used for water washing. The operation is the same as the solid-liquid separation operation of the discharge, and the discharge valve 20 is opened. The washing liquid enters the alkali solution washing tank 13, and the washing liquid is collected through the bottom discharge valve 20.
[0020] Example 2 refer to Figure 1 and Figure 3 Example 2 is described. This embodiment further describes Example 1, including an alkali solution washing tank 13 on the right side of the filter 11, an alkali solution buffer tank 14 on the side of the alkali solution washing tank 13 away from the filter 11, a second reactor 18 on the right side of the alkali solution buffer tank 14, a second circulating oil bath 17 and the filter 11 are connected to the bottom of the second reactor 18 through a pipeline 3, an acid storage tank 19 is connected to the upper end of the second reactor 18 through a pipeline, and an acid washing tank 21 and an acid storage tank 22 are connected to the right side of the second reactor 18 through pipelines. The acid buffer tank 22, the acid washing tank 21 and the pipeline 3 between the acid buffer tank 22 and the second reactor 18 are provided with a plurality of discharge valves 20 for regulation. The pipeline 3 between the first reactor 1 and the second reactor 18 is connected with an air compressor 16. The pipeline 3 on one side of the air compressor 16 is provided with a pressure regulating valve 15 for regulating the air compressor 16. The second reactor 18 is made of high borosilicate glass for storing liquid and reaction. The acid washing tank 21 and the acid buffer tank 22 are both made of corrosion-resistant PE. Among them: the alkali buffer tank 14 and the acid buffer tank 22 in this scheme are both equipped with a discharge valve 20, and this scheme is expressed by the discharge valve 20; similarly, the devices in this scheme are connected by connecting pipes 3; In this embodiment, the discharge valve 20 at the bottom of the alkali solution buffer tank 14 is manually opened, the feed liquid in the kettle is added to the kettle by controlling the flow rate of the peristaltic pump 5, the acid in the acid storage tank 19 is added to the kettle by controlling the flow rate of the peristaltic pump 5, the second circulating oil bath 17 is opened, the heating temperature is set, the kettle R02 jacket is heated, the reaction is completed, and the temperature is naturally reduced to below 50°C, the discharge valve 20 at the bottom of the second reactor 18 is manually opened, the feed liquid enters the filter 11, the air compressor 16 is turned on, the vent valve 20 of the filter 11 is closed, the pressure regulating valve 15 is adjusted, and the valve is opened. Solid-liquid separation is carried out, and the solid is retained in the filter 11. The quick release at the bottom of the filter is opened to collect the solid material, and the liquid enters the acid buffer tank 22; the discharge valve 20 at the bottom of the acid buffer tank 22 can be opened to introduce the liquid in the acid buffer tank 22 into the filter 11 for secondary filtration; water washing: the solenoid valve 9 is opened, and the water in the clean water tank 10 is added to the kettle through the peristaltic pump 5, and the jacket 32 is used for heating by the waste heat, and water washing is carried out, and the discharge valve 20 is opened, and the washing liquid enters the acid washing tank 21 and is collected through the bottom discharge valve 20.
[0021] In specific applications, in this embodiment, 500g of solid material MOCVD slag treated by a roasting furnace is added to the first reactor 1 through the solid feeding port of the first reactor 1, and 5L of alkali solution is added to the first reactor 1 by controlling the flow rate of the peristaltic pump 5 in the alkali solution storage tank 6, and the first circulating oil bath 12 is opened, and the heating temperature is set to 80°C, and the jacket 32 of the first reactor 1 is heated; wherein the non-condensable steam in the first reactor 1 can be used for tail gas absorption treatment through the absorption tank; after the reaction is completed, the temperature naturally drops to below 50°C, and the bottom of the first reactor 1 is manually opened. The bottom valve and the top valve of the filter 11 are opened, and the discharge valve of the filter 11 is closed to allow the feed liquid to enter the filter; the air compressor 16 is turned on to pressurize the filter 11, the vent valve 8 of the filter 11 is closed, and the pressure regulating valve 15 is adjusted. The valve of the alkali solution buffer tank 14 is opened to separate the solid and the liquid. The solid is trapped in the filter 11. The quick release at the bottom of the filter 11 is opened to collect the solid material, and the liquid enters the alkali solution buffer tank 14; the discharge valve 20 at the bottom of the alkali solution buffer tank 14 is manually opened, and the feed liquid in the kettle is added to the kettle by controlling the flow rate of the peristaltic pump 5, and the acid in the acid storage tank 19 is passed through 5L is added to the kettle by controlling the flow rate of the peristaltic pump 5, the second circulating oil bath 18 is turned on, the heating temperature is set to 80°C, the jacket of the blending kettle is heated, the pH value is adjusted to 3-4, the reaction is completed, gallium is precipitated, the solid-liquid mixture containing gallium is introduced into the secondary filter, filtration and washing are completed, gallium hydroxide is obtained, and the temperature is naturally reduced to below 50°C, the bottom glass valve of the kettle is manually opened, the feed liquid enters the filter 11, the air compressor 16 is turned on, the discharge valve 20 of the filter 11 is closed, the pressure regulating valve 15 is adjusted, and the valve is opened for solid-liquid separation, and the solid is trapped in the filter. 11, open the quick release at the bottom of the filter to collect solid materials, and the liquid enters the acid buffer tank 22; after the reaction is completed, water washing is carried out, and the solenoid valve 9 is opened. The water in the acid washing tank 21 is added to the kettle through peristalsis, and the waste heat of the jacket 32 is used for heating. Water washing is carried out, and the valve is opened. The washing liquid enters the acid washing tank 21, and the washing liquid is collected through the bottom discharge valve 20. The equipment operates stably, the process technology is reasonable and reliable, the ion concentrations of the leaching solution and the pH adjusting solution are stable, and the recovery rates of indium and gallium reach 99.98% and 91.4%, respectively.
[0022] In the description of the present invention, it should be noted that the orientations or positional relationships indicated by the terms "top", "bottom", "one side", "the other side", "front", "back", "middle part", "inside", "top end", "bottom end", etc. are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention; the terms "first", "second", and "third" are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance; in addition, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it 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 it can be an indirect connection through an intermediate medium, or it can be a connection between the two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0023] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.
Claims
1. LED gallium indium recycling device, characterized in that: The invention comprises a first reactor (1), wherein the first reactor (1) has an upper end connected to a pipeline (3), the other side of the pipeline (3) is connected to a condenser (2), the other side of the condenser (2) is connected to a Monteggia washing bottle (4) through a pipeline, one side of the first reactor (1) is connected to an atmosphere box-type protection electric furnace (23), the lower side of the first reactor (1) is connected to a filter (11), the outer layer of the first reactor (1) is provided with a jacket (32), the lower end of the first reactor (1) is provided with a first circulating oil bath (12), the jacket (32) and the first circulating oil bath (12) are connected to the first reactor (1), and the first reactor (1) is provided with a first circulating oil bath (12). A first circulating oil bath (12) is connected to the first reactor (1); a reduction motor (28) is provided above the first reactor (1); a stirring shaft (29) is installed at the output end of the reduction motor (28); the stirring shaft (29) is connected to the first reactor (1); an alkali liquid storage tank (6) is provided on the right side of the first reactor (1); a clean water tank (10) is provided on the right side of the alkali liquid storage tank (6); the alkali liquid storage tank (6) and the clean water tank (10) are both connected to the first reactor (1) by a pipeline (3); and a temperature sensor (30) and a sensor (31) are also provided in the first reactor (1).
2. The LED gallium-indium recycling device according to claim 1, characterized in that: An alkali solution washing tank (13) is provided on the right side of the filter (11); an alkali solution buffer tank (14) is provided on the side of the alkali solution washing tank (13) away from the filter (11); a second reactor (18) is provided on the right side of the alkali solution buffer tank (14); the bottom end of the second reactor (18) is connected to a second circulating oil bath (17) and the filter (11) via pipelines (3), respectively; and the upper end of the second reactor (18) is connected to an acid storage tank (19) via pipelines.
3. The LED gallium-indium recycling device according to claim 2, characterized in that: The right side of the second reactor (18) is connected to an acid washing tank (21) and an acid buffer tank (22) through pipelines, and a plurality of discharge valves (20) are provided on the pipelines (3) between the acid washing tank (21) and the acid buffer tank (22) and the second reactor (18) for control.
4. The LED gallium-indium recycling device according to claim 2, characterized in that: An air compressor (16) is connected to the pipeline (3) between the first reaction kettle (1) and the second reaction kettle (18), and a pressure regulating valve (15) capable of regulating the air compressor (16) is provided on the pipeline (3) on one side of the air compressor (16).
5. The LED gallium-indium recycling device according to claim 1, characterized in that: The atmosphere box-type protection electric furnace (23) is provided with an air outlet (24), the air outlet (24) is connected to the pipeline (3), a support leg (27) is fixedly installed at the bottom of the atmosphere box-type protection electric furnace (23) for supporting, a rotor flow meter (25) is provided on one side of the atmosphere box-type protection electric furnace (23), and a control panel (26) is installed in the atmosphere box-type protection electric furnace (23) for controlling.
6. The LED gallium-indium recycling device according to claim 1, characterized in that: A solenoid valve (9) is installed between the first reaction kettle (1) and the clean water tank (10), and a peristaltic pump (5) is provided between the first reaction kettle (1) and the alkali solution storage tank (6), wherein a feeding valve (7) and a drain valve (8) are respectively installed on the alkali solution storage tank (6), and the feeding valve (7) and the drain valve (8) are symmetrically arranged on both sides of the alkali solution storage tank (6).
7. The LED gallium-indium recycling device according to claim 1, characterized in that: A stirring blade (33) is fixedly mounted on the bottom end of the stirring shaft (29), and an interface (34) is mounted on the bottom end of the first reaction kettle (1), wherein the interface (34) is connected to the pipeline (3).
8. The LED gallium-indium recycling device according to claim 1, characterized in that: The alkali solution storage tank (6), the first reaction kettle (1), the alkali solution washing tank (13) and the alkali solution buffer tank (14) are all made of 316L stainless steel.
9. The LED gallium-indium recycling device according to claim 2, characterized in that: The second reaction kettle (18) is made of high borosilicate glass material for storing liquid and for reaction, and the acid washing tank (21) and the acid buffer tank (22) are both made of corrosion-resistant PE material.
10. The LED gallium-indium recycling device according to claim 1, characterized in that: The working chamber volume of the atmosphere box-type protection electric furnace (23) is 8L, the maximum temperature is 1200°C, and a gas outlet (24) is provided on the front side, wherein the waste gas is connected to the Monteggia washing bottle (4) through a pipeline (3) for waste gas adsorption treatment.