An environmentally friendly high-purity indium continuous purification device

Abstract

The invention relates to an environmentally friendly high-purity indium continuous purification device, comprising an indium purification device furnace body, an indium raw material feeding furnace, a high-purity indium product discharging furnace, an indium medium-low boiling point collecting furnace, and an indium continuous purification residue collecting furnace. The indium purification device furnace body is used for vacuum distillation purification of raw material indium. The indium raw material feeding furnace is connected to the lower section of the indium purification device furnace body through a pipeline, and has an independent vacuum system and a raw material indium processing device. The high-purity indium product discharging furnace is connected to the upper section of the indium purification device furnace body through a pipeline, and has a product indium collecting device. The indium medium-low boiling point collecting furnace is connected to the upper section of the indium purification device furnace body through a pipeline, and has a low boiling point collecting device. The indium continuous purification residue collecting furnace is connected to the lower section of the indium purification device furnace body through a pipeline, and has a residue collecting device after indium purification. The device of the present invention is used for continuous purification of high-purity indium, has high production efficiency, good product quality, low production cost, no toxic and harmful gas emissions, and meets the quality and environmental protection requirements of high-purity indium preparation.

Description

Technical Field

[0001] The invention relates to the field of high-purity indium production equipment, and in particular to an environmentally friendly high-purity indium continuous purification and preparation device. Background Art

[0002] Indium metal is a soft silvery-white metal. It has excellent physical and chemical properties such as strong metallic luster, good ductility, strong plasticity, low melting point and high boiling point, good light permeability and conductivity, and corrosion resistance. High-purity indium is a key basic material for the production of copper indium gallium selenide thin-film solar cells (CIGS) and semiconductor materials (indium phosphide, indium antimonide, etc.). In the semiconductor industry, high-purity indium is mainly used as a raw material for III-V semiconductor materials, and reacts with Ga, P, Sb, etc. to make a single semiconductor device. In recent years, high-purity indium has been widely used in high-tech fields such as solar photovoltaic, flat-panel liquid crystal display, national defense and military, aerospace, optical communications, and electronic information industries. The purity of indium metal directly affects the physical and chemical properties of the material. The subsequent materials prepared by indium of different purities are used in different fields. For example, 99.99% and 99.999% indium are mainly used to prepare ITO targets and CIGS, 6N indium is mainly used to prepare indium phosphide and indium antimonide compound semiconductor materials, and 99.99999% and above purity indium is mainly used for MBE and special alloys. With the vigorous development of high-tech in the fields of new energy, optoelectronics, aerospace, national defense and military, the demand for high-purity indium is increasing.

[0003] At present, there are mainly the following methods for purifying high-purity indium:

[0004] Sublimation method

[0005] Sublimation purification mainly uses the sublimation of In2O or InCl to purify metallic indium. -4 Pa vacuum conditions, and then heat and melt it, and keep it at 800℃ for 5 hours for sublimation, to complete the purification of indium. The sublimation method has a good purification effect on indium, but the equipment is expensive and is only suitable for processing a small amount of samples.

[0006] Electrolytic refining

[0007] At present, enterprises producing 4N refined indium in my country mainly adopt electrolytic refining. Electrolytic refining is difficult to remove elements with a potential close to that of indium, such as cadmium and thallium. And elements with a potential more negative than indium, such as zinc and lead, dissolve in the electrolyte and accumulate in the electrolyte, polluting the electrolyte. Therefore, it is difficult to remove cadmium and thallium during the electrolysis of crude indium, and zinc, lead, cadmium, thallium, etc. will pollute the electrolyte, increasing the difficulty and cost of electrolyte purification.

[0008] Zone Melting

[0009] Zone melting is a method that utilizes the difference in solubility of metals in solidified and molten states to precipitate impurities or change their distribution. By locally heating a narrow ingot, one or several narrow melting zones are formed in the ingot, and then the heater is slowly moved to make this narrow melting zone move slowly along the ingot in a certain direction. Due to the difference in equilibrium concentration of impurities in the solid phase and liquid phase, the impurities are segregated into the solid phase or liquid phase during repeated melting and solidification, thereby purifying the main metal.

[0010] Vacuum distillation

[0011] The vacuum distillation method uses the difference in saturated vapor pressure of each impurity element in crude indium to control the appropriate distillation temperature, so that each impurity element can be selectively volatilized and condensed, and enriched in the volatilized gas phase and the residual liquid phase, respectively, so as to purify the metallic indium. The vacuum distillation purification of metallic indium is carried out in a vacuum heating furnace. The entire purification process is a physical change, with simple operation, short process flow, and easy automation. In addition, no wastewater, waste gas, or waste residue is generated during the entire purification process, which causes very little pollution to the environment. It is a green and environmentally friendly purification method.

[0012] The development of my country's indium industry started late, and the indium industry still has many problems such as unbalanced development and incomplete structure. For example, the output of indium ingots is large, but the usage is small; the main production is crude indium and refined indium, and the industrialization and industrialization of deep-processing products have not made breakthrough progress; high-tech and high-value-added products such as high-purity indium, ITO targets, and indium-containing semiconductor materials have not been able to form market competitiveness, and the output is very small, and a large amount needs to be imported from abroad.

[0013] Therefore, it is necessary to study an environmentally friendly high-purity indium continuous purification device to meet the demand for raw materials in the preparation process of high-purity indium, and also meet the needs of the development of the semiconductor industry. However, there is no related equipment for environmentally friendly high-purity indium continuous purification in the currently available information. Therefore, the development of an environmentally friendly high-purity indium continuous purification device can meet the needs of high-purity indium purification, improve production efficiency, and reduce environmental pollution during the purification process. Summary of the invention

[0014] In order to solve the above technical problems, the present invention provides an environmentally friendly high-purity indium continuous purification device, which can improve the preparation efficiency of high-purity indium, reduce labor intensity, and improve the quality of the prepared high-purity indium; at the same time, the device is in a relatively sealed environment when working, and low-boiling point toxic and harmful substances are recycled and processed, which can effectively reduce the emission of toxic and harmful gases in the preparation process; meet the demand for high-purity indium in the high-purity indium demand industry and the environmental protection requirements in the process of purifying high-purity indium.

[0015] The technical solution adopted by the present invention to solve its technical problems is: an environmentally friendly high-purity indium continuous purification device, including an indium purification device furnace body, an indium raw material feeding furnace, a high-purity indium product discharging furnace, an indium medium and low boiling point collection furnace, and an indium continuous purification residual material collection furnace. A closed furnace chamber is formed inside the indium purification device furnace body, and a heat preservation system is provided in the furnace chamber. The lower part of the furnace chamber is the evaporation zone of the furnace body, which is used for vacuum distillation of raw material indium. The middle part of the furnace chamber is the product collection zone of the furnace body, which is used for collecting liquid high-purity indium products; the upper part of the furnace chamber is the low boiling point collection zone in the distillation process of the furnace body, which is used for collecting low boiling points in the distillation process; an indium raw material distillation crucible is installed in the evaporation zone for storing raw material indium; a product collection crucible and an indium steam condensation device are installed in the product collection zone; a low boiling point collection crucible and a low boiling point condensation device are installed in the low boiling point collection zone. The indium raw material feeding furnace is an independent closed cavity, and an independent vacuum system and raw material indium processing device are provided on the cavity. The raw material processing device is connected to the lower section of the indium purification device furnace body through a pipeline. The high-purity indium product discharge furnace is an independent cavity, and there is a product indium collection device in the cavity, which is connected to the upper part of the indium purification device furnace body through a pipeline. The indium medium and low boiling point collection furnace is an independent cavity, and there is a low boiling point collection device in the cavity, which is connected to the upper part of the indium purification device furnace body through a pipeline. The indium continuous purification residue collection furnace is an independent cavity, and there is a residue collection device after indium purification in the cavity, which is connected to the lower part of the indium purification device furnace body through a pipeline.

[0016] Furthermore, two groups of lower-section heating electrodes and a set of heating devices are provided on the outer side of the furnace body of the indium purification device at a position corresponding to the evaporation zone, the lower section is provided with a temperature-controlling thermocouple, and the heating device cooperates with the lower-section temperature-controlling thermocouple to adjust the temperature of the evaporation zone in the lower section of the furnace body; two groups of upper-section heating electrodes and a set of heating devices are provided on the outer side of the upper section of the furnace body at a position corresponding to the product condensation zone, the upper section is provided with a temperature-controlling thermocouple, and the heating device cooperates with the upper-section temperature-control thermocouple to adjust the temperature of the product condensation zone in the upper section of the furnace body.

[0017] Furthermore, the indium raw material feeding furnace is provided with a heating device and a temperature control thermocouple, and the heating device cooperates with the temperature control thermocouple to adjust the temperature in the raw material feeding furnace. The raw material feeding furnace is also provided with an indium raw material storage crucible for storing the melted raw material indium liquid.

[0018] Furthermore, a heating device and a temperature-controlling thermocouple are provided in the high-purity indium product discharge furnace, and the heating device cooperates with the temperature-controlling thermocouple to adjust the temperature in the high-purity indium product discharge; the high-purity indium product furnace is also provided with a high-purity indium product weighing device, which is used to weigh the collected high-purity indium product weight in order to determine the discharge time.

[0019] Furthermore, a low-boiling-point collecting crucible is provided in the indium low-boiling-point collecting furnace for collecting low-boiling-point materials, and the low-boiling-point materials are periodically discharged from the furnace according to the collection conditions.

[0020] Furthermore, a distillation residue collecting crucible is provided in the indium continuous distillation residue collecting furnace, which is used to collect the residue after distillation, and the residue is removed from the furnace regularly according to the collection situation of the residue.

[0021] Furthermore, an automatic control valve is provided on the pipeline of the indium raw material feeding furnace, and the automatic control valve is used in conjunction with the PLC operation interface on the control screen to adjust the operation of the automatic control valve according to the set parameters.

[0022] Furthermore, the high-purity indium product discharging device is used in conjunction with a high-purity indium product discharging control valve to control the opening and closing operation of the valve according to a set weighing weight.

[0023] Furthermore, the control module forms a communication connection with the upper temperature-controlled thermocouple, the lower temperature-controlled thermocouple, the indium raw material feed control valve, the high-purity indium product discharge control valve, the indium medium and low-boiling material discharge control valve, the indium continuous purification residue discharge control valve, the heating component, the insulation and heating component, and the high-purity indium product weighing device.

[0024] Furthermore, a furnace cover is arranged on the top side of the furnace body, and the furnace cover is fixed to the furnace body by fasteners; and a vacuum extraction device is installed on the furnace body.

[0025] Furthermore, the pipelines are provided with heat tracing and heat preservation devices for heating the pipelines.

[0026] Advantages of the present invention: The environmentally friendly high-purity indium continuous purification device of the present invention integrates the distillation and purification of high-purity indium and the vapor-liquid exchange of indium vapor and indium liquid in the main furnace body, and is also equipped with a continuous raw material feeding furnace and a continuous product discharging furnace, thereby realizing continuous operation in the high-purity indium purification process. The device is also provided with a centralized collection and post-processing of low-boiling substances in indium, which can effectively avoid the emission of toxic and harmful substances in the preparation process of high-purity indium, and reduce the material loss in the preparation process of high-purity indium. The high-purity indium continuous purification device solves the problem that in the conventional purification process of high-purity indium, the temperature needs to be lowered to room temperature after purification of one batch, and then the furnace needs to be opened and discharged before the next batch of purification operations are carried out, thereby improving production efficiency and reducing energy consumption in the purification process.

[0027] The heating device installed in the indium raw material evaporation zone and the indium steam condensation zone can effectively control the temperature field control of the evaporation zone and the condensation zone, which can meet the requirements of the indium purification effect, and can achieve the purification of the indium raw material with a purity of about 99.995% to 99.9999% at one time. The low-boiling point collection device in the indium distillation and purification process is used to collect the low-boiling points in a liquid form after condensation, and the toxic and harmful gases and dust in the furnace will not escape into the environment. In the design of the indium raw material feeding device, an automatic interlocking control valve is set on the feeding pipeline to realize the automation and continuity of the feeding, and ensure the continuous purification of high-purity indium. The high-purity indium discharging device is equipped with a product collection and weighing device on the product crucible. The weighing device is interlocked with the automatic valve on the product discharging pipeline, which can not only realize the continuity of the product discharging, but also determine the distillation of the raw indium in the evaporation zone according to the weight of the discharging. The control module receives the monitoring data of each sensor, and controls the opening or closing of each valve according to the monitoring data. The degree of automation control is high, the labor intensity is low, the production efficiency is high, and the safety and environmental protection are good. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a schematic diagram of an environmentally friendly high-purity indium continuous purification device according to Example 1;

[0029] Figure 2 This is a schematic diagram of the internal structure of an environmentally friendly high-purity indium continuous purification device according to Example 1;

[0030] Figure 3 This is a schematic diagram of a high-purity indium product collecting crucible in a product discharge furnace in an environmentally friendly high-purity indium continuous purification device in Example 1.

[0031] Among them: 1-indium continuous purification device support; 2-indium continuous purification device furnace; 21-furnace lower section heating device; 211-lower section heating 1# electrode; 212-lower section heating 2# electrode; 213-lower section heating temperature control couple; 22-furnace upper section heating device; 221-upper section heating 1# electrode; 222-upper section heating 2# electrode; 223-upper section heating temperature control couple; 23-purification device furnace body sealing cover; 231-device sealing cover opening device; 24, purification device internal parts; 241-indium raw material distillation crucible; 242-high purity indium product collection device; 243-high purity indium steam condensation device; 244-indium medium and low boiling point collection device; 245-indium medium and low boiling point condensation device; 25-indium continuous purification device vacuum system; 3-indium raw material feeding furnace; 31-indium raw material feeding furnace vacuum device; 32-indium raw material feeding pipe; 33-indium raw material feeding control valve; 34-indium raw material chemical device; 35-feeding furnace temperature control couple; 4-high-purity indium product discharging furnace; 41-product discharging furnace vacuum device; 42-high-purity indium product discharging pipe; 43-high-purity indium product discharging control valve; 44-high-purity indium product collecting device; 45-high-purity indium product weighing device; 46-product discharging furnace temperature control couple; 5-indium medium and low boiling point collecting furnace; 51-indium medium and low boiling point discharging pipe; 52-indium medium and low boiling point discharging control valve; 53-indium medium and low boiling point collecting device; 6-indium continuous purification residue collecting furnace; 61-residue discharging pipe; 62-residue discharging control valve; 63-residue collecting device. Implementation

[0032] In order to deepen the understanding of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. The embodiments are only used to explain the present invention and do not limit the protection scope of the present invention. Example

[0033] Please refer to Figure 1 , Figure 2 and Figure 3As shown, this embodiment provides an environmentally friendly high-purity indium continuous purification device, including an indium purification device furnace body 2, an indium raw material feeding furnace 3, a high-purity indium product discharging furnace 4, an indium medium and low boiling point collection furnace 5 and an indium continuous purification residue collection furnace 6. The furnace body 2 of the indium purification device is installed on the bracket 1 of the indium continuous purification device, and a closed furnace cavity is formed inside. The furnace cavity is provided with a heat preservation system. The lower part of the furnace cavity is the evaporation zone of the furnace body. The evaporation zone is provided with a furnace lower section heating device 21. The furnace lower section heating device 21 has lower section heating electrodes 212 and 213, and is also provided with a lower section heating temperature control couple 213. The furnace lower section heating device 21 is used for vacuum distillation of raw material indium. The middle part of the furnace cavity is a high-purity indium product collecting device 242 and a high-purity indium steam condensing device 243 of the furnace body, which are used to collect liquid high-purity indium products; and are used to collect low-boiling substances in the distillation process; an indium raw material distillation crucible 241 is installed in the evaporation zone for storing raw material indium; a low-boiling substance collecting device 244 and a low-boiling substance condensing device 245 are installed in the low-boiling substance collecting device 243. The indium raw material feeding furnace 3 is an independent closed cavity, and an independent vacuum system 31 and a raw material indium material device 34 are arranged on the cavity. The raw material indium material device 34 is connected to the lower section of the furnace body 2 of the indium purification device through an indium raw material feeding pipe 32. The high-purity indium product discharging furnace 4 is an independent cavity, and a product indium collecting device 44 is arranged in the cavity, and the high-purity indium product discharging furnace 4 is connected to the upper section of the furnace body 2 of the indium purification device through a high-purity indium product discharging pipe 42. The indium medium and low boiling point collecting furnace 5 is an independent cavity, and a low boiling point collecting device 53 is arranged in the cavity, and the indium medium and low boiling point collecting furnace 5 is connected to the upper section of the furnace body 2 of the indium purification device through an indium medium and low boiling point discharging pipe 51. The indium continuous purification residue collecting furnace 6 is an independent cavity, and a residue collecting device 63 is arranged in the cavity, and the indium continuous purification residue collecting furnace 6 is connected to the lower section of the furnace body 2 of the indium purification device through a residue discharging pipe 61.

[0034] Refer to Figure 1 The outer side of the furnace body 2 of the indium purification device is provided with two groups of lower heating electrodes 211 and 212 at a position corresponding to the evaporation zone, and a set of heating device 21, the lower section is provided with a temperature-controlling electric couple 213, and the heating device 21 cooperates with the lower section temperature-controlling electric couple 213 to adjust the temperature of the lower section evaporation zone of the furnace body; the outer upper section of the furnace body is provided with two groups of upper heating electrodes 221 and 222 at a position corresponding to the product condensation zone, and a set of heating device 22, the upper section is provided with a temperature-controlling electric couple 223, and the heating device 22 cooperates with the upper section temperature-controlling electric couple 223 to adjust the temperature of the upper section product condensation zone of the furnace body.

[0035] Refer to Figure 1 and Figure 2The indium raw material feeding furnace 3 is provided with a heating device and a feeding furnace temperature control couple 35. The heating device cooperates with the temperature control couple 35 to adjust the temperature in the raw material feeding furnace. An independent indium raw material feeding furnace vacuum device 31 is also provided. The raw material feeding furnace 3 is also provided with an indium raw material quenching device 34 for storing the melted raw material indium liquid. The indium raw material feeding pipe 32 is provided with a feeding control valve 33. The feeding pipe 32 is connected to the raw material distillation crucible 241 at the lower part of the furnace body 2 of the indium purification device.

[0036] Refer to Figure 1 The high-purity indium product discharging furnace 4 is provided with a heating device and a discharging furnace temperature-controlling couple 46. The heating device cooperates with the discharging furnace temperature-controlling couple 46 to adjust the temperature of the high-purity indium product discharging. At the same time, an independent product furnace vacuum device 31 is also provided; the high-purity indium product furnace 4 is also provided with a high-purity indium product weighing device 45 to weigh the collected high-purity indium product weight. The high-purity product weighing device 45 is used to determine the discharging time. A product discharging control valve 43 is provided on the product discharging pipeline 42. The product discharging control valve 43 cooperates with the product weighing device 45. When the set weight is reached, the discharging control valve 43 is automatically closed. The product discharging pipe 42 is connected to the high-purity indium product collecting device 242 in the middle of the furnace body 2 of the indium purification device.

[0037] Refer to Figure 1 A low-boiling-point material collecting device 53 is provided in the indium low-boiling-point material collecting furnace 5, which is used to collect low-boiling-point materials. According to the collection situation of the low-boiling-point materials, the furnace is discharged regularly. A low-boiling-point material discharge control valve 52 is provided on the indium low-boiling-point material discharge pipe 51 for controlling the outflow of low-boiling-point materials. The indium low-boiling-point material discharge pipe 51 is connected to the low-boiling-point material collecting device 53 on the upper part of the furnace body 2 of the indium purification device.

[0038] Refer to Figure 1 The indium continuous distillation residue collection furnace 6 is provided with a distillation residue collection device 63, which is used to collect the residue after distillation. According to the collection situation of the residue, the furnace is regularly discharged to reduce the loss of indium during the purification process, and at the same time, a small amount of indium and indium vapor during the purification process is avoided from entering the furnace or the exhaust pipe.

[0039] Refer to Figure 1 The indium raw material feeding pipe 32 of the indium raw material feeding furnace 3 is provided with an automatic control valve 33, which is used in conjunction with the PLC operation interface on the control screen to adjust the operation of the automatic control valve according to the set parameters.

[0040] Refer to Figure 1The control module is connected to the upper temperature-controlled thermocouple 223, the lower temperature-controlled thermocouple 213, the indium raw material feed control valve 33, the high-purity indium product discharge control valve 43, the indium medium and low boiling point discharge control valve 52, the indium continuous purification residual material discharge control valve 62, the heating component 21, the insulation and heating component, and the high-purity indium product weighing device 45 to form a communication connection.

[0041] Refer to Figure 1 A purification device furnace body sealing cover 23 is provided on the top of the furnace body, and the purification device furnace body sealing cover 23 is fixed to the indium purification device furnace body 2 through a device sealing device 231; an indium continuous purification device vacuum system 25 is installed on the indium purification device furnace body 2.

[0042] Refer to Figure 1 The pipelines are all equipped with heat tracing and heat preservation devices for heating the indium raw material feed pipe 32, the high-purity indium product discharge pipe 42, the indium medium and low boiling point discharge pipe 51 and the purified residual material discharge pipe 61.

[0043] Refer to Figure 2 and Figure 3 The internal shape and size of the indium raw material crucible 241 can be designed according to actual needs so that the high-purity indium after distillation and purification can reach the required external dimensions. Example

[0044] This embodiment provides a method for preparing high-purity indium with a purity of 99.9999% using an environmentally friendly high-purity indium continuous purification device, which is specifically carried out in the following steps:

[0045] S1. Prepare a raw material indium ingot with a purity of about 99.995%. The size of the indium ingot is smaller than the size of the indium raw material crucible, and set aside;

[0046] S2. Open the furnace sealing cover on the furnace body of the indium continuous purification device, and sequentially load the indium raw material distillation crucible, the high-purity indium product collecting device, the high-purity indium steam condensing device, the indium medium and low boiling point collecting device and the low boiling point condensing device, then close the sealed furnace cover and lock it, open the vacuum system on the furnace body to evacuate the vacuum, and at this time, the valves on each pipeline are in a closed state;

[0047] S3, then open the high-purity indium product discharging furnace, the indium medium and low boiling point collection furnace and the indium continuous purification residue collection furnace, respectively load the high-purity indium product collection crucible, the indium medium and low boiling point collection crucible and the residue collection crucible, finally seal the furnace body and start the vacuum device on each furnace body;

[0048] S4. Open the door of the indium raw material feeding furnace, put in the indium raw material crucible, load 50-100 kg of raw indium, seal the furnace body, and start the vacuum system to evacuate to 10 -1Pa, turn on the material heating device of the feed furnace, set the heating temperature to 250°C-350°C to melt the indium raw material;

[0049] S5. Wait until the vacuum value in the furnace of the indium purification device reaches 10 -2 When Pa, the feed control valve is opened to allow the indium raw material in the feed furnace to flow into the distillation crucible in the purification device. After the indium raw material in the feed furnace has flowed out, the feed control valve is closed, and the heating devices of the upper and lower sections of the furnace body are turned on. The heating temperature of the upper section is set to 980°C-1080°C, and the heating temperature of the lower section is set to 1120°C-1200°C. After the temperatures are reached, the purification operation of indium is carried out;

[0050] S6. After the indium purification operation is carried out for 30-60 minutes, open the product discharge pipe control valve to continuously discharge the high-purity indium product. After the purification operation is carried out continuously for 20-40 hours, open the control valve on the residual material discharge pipe and the control valve on the low-boiling material discharge pipeline respectively. The discharge time is 10-20 minutes. After the discharge operation is completed, close the above control valves. The operation of this step is completed automatically according to the program set on the PLC control system;

[0051] S7. The crucible mold for receiving materials in the high-purity indium product discharge furnace is designed according to the size and weight required by the customer or the downstream re-purification process, and the control weight of the weighing device is set according to the required weight to control the discharge valve;

[0052] S8, repeat step S4 to complete the secondary feeding. During the feeding process, the vacuum degree and temperature in the furnace of the indium purification device remain unchanged according to the set values. After the feeding is completed, the indium purification operation continues;

[0053] S9: The subsequent purification operation repeats the operation of step S6 according to the set program.

[0054] S10. After the continuous purification of indium has been running for 5-8 days, the material treatment operation in the residual material collection furnace and the low-boiling-point collection furnace is carried out.

[0055] In this embodiment, the preparation process is always carried out in a closed environment, and the toxic and harmful exhaust gas generated enters the low-boiling-point collection system, and no harmful gas leaks out; the purification process can realize the continuous purification of indium, the purification efficiency of high-purity indium is high, and the quality of the purified high-purity indium product is better than 99.9999%, and the degree of automation is high, the operation is simple, the labor intensity is low, and one person can complete the operation independently.

[0056] Comparative Example 1

[0057] The difference between this comparative example and the first embodiment is that in step S3, there is no indium raw material feeding furnace and product discharging furnace, and the rest is the same as the first embodiment.

[0058] In this comparative example, the continuity of the indium purification process cannot be achieved, and each batch needs to be unloaded from the furnace, and after each batch of purification is completed, the temperature needs to be lowered for at least 10 hours before it can be unloaded from the furnace, and the temperature needs to be raised again after loading. This results in low purification efficiency, high energy consumption, and high production costs.

[0059] Comparative Example 2

[0060] The difference between this comparative example and the first embodiment is that in step S6, no low-boiling-point collecting device is designed. The rest is the same as the first embodiment.

[0061] In this comparative example, there is a pungent smell every time the furnace door is opened, and there is a large amount of powder in the indium purification furnace, which requires regular cleaning of the interior of the furnace; the loss in the indium purification process reaches 3-5% (when there is a low-boiling point collection device, the loss in the purification process is less than 2%).

[0062] Comparative Example 3

[0063] The difference between this comparative example and the first embodiment is that in step S7, the crucible for collecting the high-purity indium product is a conventional barrel-shaped crucible. The rest is the same as the first embodiment.

[0064] In this comparative example, the collected high-purity indium product needs to be melted again and then cast into ingots of the size required by the customer or downstream re-purification process, thereby increasing the loss in the casting process by about 0.5% and also increasing the labor intensity.

[0065] The above embodiments should not limit the present invention in any way, and any technical solutions obtained by equivalent replacement or equivalent conversion shall fall within the protection scope of the present invention.

Claims

1. An environmentally friendly high-purity indium continuous purification device, characterized in that: The invention comprises a furnace body of an indium purification device, an indium raw material feeding furnace, a high-purity indium product discharging furnace, an indium medium- and low-boiling-point collecting furnace, and an indium continuous purification residue collecting furnace; a closed furnace chamber is formed inside the furnace body of the indium purification device, and a heat preservation system is arranged in the furnace chamber; the lower part of the furnace chamber is an evaporation zone of the furnace body, which is used for vacuum distillation of raw indium; the middle part of the furnace chamber is a product collecting zone of the furnace body, which is used for collecting liquid high-purity indium products; the upper part of the furnace chamber is a low-boiling-point collecting zone in the distillation process of the furnace body, which is used for collecting low-boiling-points in the distillation process; an indium raw material distillation crucible is installed in the evaporation zone for storing raw indium; and a Equipped with a product collecting crucible and an indium vapor condensing device; a low-boiling-substance collecting crucible and a low-boiling-substance condensing device are installed in the low-boiling-substance collecting area; the indium raw material feeding furnace is an independent closed cavity, on which there are an independent vacuum system and a raw material indium processing device, and the raw material processing device is connected to the lower section of the furnace body of the indium purification device through a pipeline; the high-purity indium product discharging furnace is an independent cavity, in which there is a product indium collecting device, and the device is connected to the upper section of the furnace body of the indium purification device through a pipeline; the indium medium-low boiling-substance collecting furnace is an independent cavity, in which there is a low-boiling-substance collecting device, and the device is connected to the upper section of the furnace body of the indium purification device through a pipeline; The indium continuous purification residue collection furnace is an independent cavity, and a residue collection device after indium purification is arranged in the cavity, and the device is connected to the lower section of the furnace body of the indium purification device through a pipeline; two groups of lower section heating electrodes and a set of heating devices are arranged at the outer side of the furnace body of the indium purification device at a position corresponding to the evaporation zone, the lower section is provided with a temperature control thermocouple, and the heating device cooperates with the lower section temperature control thermocouple to adjust the temperature of the evaporation zone of the lower section of the furnace body; two groups of upper section heating electrodes and a set of heating devices are arranged at a position corresponding to the product condensation zone of the outer side of the furnace body, the upper section is provided with a temperature control thermocouple, and the heating device cooperates with the upper section temperature control thermocouple to adjust the temperature of the product condensation zone of the upper section of the furnace body.

2. An environmentally friendly high-purity indium continuous purification device according to claim 1, characterized in that: The indium raw material feeding furnace is provided with a heating device and a temperature-controlling thermocouple, and the heating device cooperates with the temperature-controlling thermocouple to adjust the temperature in the raw material feeding furnace; the raw material feeding furnace is also provided with an indium raw material storage crucible for storing melted raw material indium liquid.

3. The environmentally friendly high-purity indium continuous purification device according to claim 1, characterized in that: The high-purity indium product discharge furnace is provided with a heating device and a temperature-controlling thermocouple, and the heating device cooperates with the temperature-controlling thermocouple to adjust the temperature in the high-purity indium product discharge; the high-purity indium product furnace is also provided with a high-purity indium product weighing device, which is used to weigh the collected high-purity indium product weight in order to determine the discharge time.

4. The environmentally friendly high-purity indium continuous purification device according to claim 1, characterized in that: A low-boiling-point collecting crucible is arranged in the indium low-boiling-point collecting furnace, which is used to collect low-boiling-point materials. The low-boiling-point materials are discharged from the furnace regularly according to the collection conditions.

5. The environmentally friendly high-purity indium continuous purification device according to claim 1, characterized in that: The indium continuous distillation residue collection furnace is provided with a distillation residue collection crucible for collecting the residue after distillation. The crucible is used to collect the residue after distillation and to periodically remove the residue from the furnace according to the collection status of the residue.

6. The environmentally friendly high-purity indium continuous purification device according to claim 2, characterized in that: An indium raw material feed control valve is arranged on the pipeline of the indium raw material feed furnace, and the indium raw material feed control valve is used in conjunction with the PLC operation interface on the control screen, and its function is to adjust the operation of the automatic control valve according to the set parameters.

7. The environmentally friendly high-purity indium continuous purification device according to claim 3, characterized in that: The high-purity indium product discharging furnace is used in conjunction with a high-purity indium product discharging control valve, and the valve opening and closing operation is controlled according to a set weighing weight.

8. An environmentally friendly high-purity indium continuous purification device according to any one of claims 1 to 7, characterized in that: A control module is also provided, which is connected to the upper temperature control thermocouple, the lower temperature control thermocouple, the indium raw material feed control valve, the high-purity indium product discharge control valve, the indium medium and low boiling point discharge control valve, the indium continuous purification residual material discharge control valve, the heating component, the insulation heating component, and the high-purity indium product weighing device to form a communication connection.

9. An environmentally friendly high-purity indium continuous purification device according to any one of claims 1 to 7, characterized in that: A furnace cover is arranged on the top side of the furnace body, and the furnace cover is fixed to the furnace body by fasteners; a vacuum extraction device is installed on the furnace body.

10. An environmentally friendly high-purity indium continuous purification device according to any one of claims 1 to 7, characterized in that: The pipelines are provided with heat tracing and heat preservation devices for heating the pipelines.

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