A method and equipment for self-flowing continuous segregation refined antimony smelting

Abstract

The present invention relates to the field of antimony metal smelting, and discloses a method and equipment for smelting refined antimony by self-flowing continuous segregation. The equipment includes a raw material preparation device, a continuous segregation smelting device, an output product collection device, and an auxiliary monitoring device. The method uses 95% crude antimony as raw material, and obtains 99.9% refined antimony through the steps of raw material preparation, heating and quenching, continuous condensation segregation, product collection, and tailing material collection. Compared with the existing antimony metal smelting technology, the present invention utilizes the segregation purification principle, combined with the fact that the distribution coefficient of most impurities in antimony is less than 1, to achieve efficient and continuous smelting of refined antimony under low temperature difference conditions; and the number of operating segregation bins can be adjusted according to the quality of the raw materials to ensure product quality, and has good raw material adaptability. The present invention has the advantages of simple process flow, low operating energy consumption, continuous production, and less waste.

Description

Technical Field

[0001] The present invention belongs to the technical field of smelting equipment, and particularly relates to a method and equipment for continuous gravity segregation refining of antimony. Background Art

[0002] The chemical symbol of antimony is Sb, and its atomic number is 51. It belongs to the nitrogen group elements and is located in the fifth period of the periodic table. Antimony is a silver-white metal with metallic luster, but it will gradually lose its luster in humid air, and it will burn into white antimony oxide when strongly heated. Antimony is brittle and easy to wear and break, has no ductility, poor thermal conductivity, and its conductivity is only 4.2% of that of silver. The density of antimony is 6.68 g / cm³ (20˚C), the melting point is 630 °C, and the boiling point is 1750 °C (101.325 kPa).

[0003] As a strategic metal, antimony has a wide range of applications in industry. Antimony trioxide is mainly used in the production of white pigments, paints, plastics, and flame retardants, etc.; antimony alloys, as hardeners, play an important role in the fields of metallurgy, storage batteries, and military industry, etc.; ethylene glycol antimony is used as a novel catalyst in the polyester polycondensation reaction; antimony sulfide can be used as an additive for wear-resistant materials; the main use of sodium pyroantimonate is as a glass fining agent and flame retardant synergist, which is an indispensable key material in the production of photovoltaic glass and is used to improve the color and transparency of the glass.

[0004] The smelting methods of antimony mainly include two categories: pyrometallurgy and hydrometallurgy. Pyrometallurgy is one of the most important current antimony smelting methods. This method uses stibnite or antimony sulfide ore as raw materials, heats them with a reducing agent in a reverberatory furnace to reduce antimony compounds to metallic antimony, and then distills out metallic antimony. Its advantages are: large unit production capacity; long history and mature process; can directly produce antimony compounds, etc. Its disadvantages are: high-temperature operation and poor working conditions; high energy consumption and high environmental protection cost; high requirement for ore grade, etc.

[0005] Hydrometallurgy uses stibnite or antimony sulfide ore as raw materials and electrolyzes them in an electrolytic cell to electrolyze antimony compounds into metallic antimony. Its advantages are: high metal recovery rate; can process various complex ores; relatively low energy consumption and less impact on the environment. Its disadvantages are: long process and difficult liquid-solid separation; strong corrosion to equipment and requires special anti-corrosion measures; relatively high production cost, especially in the electrolytic refining stage.

[0006] The segregation melting method is a physical method for purifying metals, including fractional crystallization method, directional solidification method, zone melting method, etc., which is widely used in the field of high-purity material preparation. Currently, it is mainly used for the smelting of refined aluminum in the field of metal smelting. This method utilizes the difference in the distribution coefficient of impurity elements between the liquid and solid phases during the solidification process of metals, enabling impurities with an equilibrium distribution coefficient less than 1 to continuously transfer and accumulate in the liquid phase, so that refined aluminum solidifies and precipitates in a relatively pure crystal sequence. This method has the advantages of low investment and low energy consumption, and has a good removal effect on impurities such as Fe, Si, Cu, and Ca in the crude aluminum melt. It is a relatively mature process for the preparation of refined aluminum and high-purity aluminum in the world today.

[0007] Chinese Patent CN206768196U discloses a device for continuous purification of refined aluminum. This method uses flowing aluminum liquid to provide purification raw materials, and cooperates with the reciprocating movement of the hydraulic tightening disc and the hydraulic traction rod to continuously produce refined aluminum. When purifying, the aluminum liquid is placed in an open purification furnace body. The liquid level and surface oxide layer of the upper-layer aluminum liquid remain relatively stable, and the oxide layer forms a relatively good protective effect on the aluminum liquid. However, it is not applicable to the purification of antimony. Because antimony is extremely easy to react with elements such as oxygen, sulfur, and nitrogen at high temperatures, and some of the substances generated by the reaction will dissolve in the antimony solution or have a density less than that of antimony. It cannot play a protective role for antimony and affects the purification effect of antimony.

[0008] Chinese Patent CN218232531U provides a device for a segregation furnace that can be continuously purified, solving the problem that the current segregation furnace has low production efficiency and cannot achieve continuity. This device uses a rotatable condensation crystallizer and an electromagnetic stirrer for purification. The device has a reasonable structure, is easy to operate, and has a high degree of automation, significantly improving production efficiency and reducing production costs. However, it cannot be used for large-scale industrial continuous production. There is no automatic feeding and discharging device, which requires a large amount of labor cost. When conducting large-scale purification, the cost of the condensation crystallizer and electromagnetic stirrer required is relatively high, and the space occupied by the furnace body is relatively large.

[0009] Chinese Patent CN113774231B provides a device for producing high-purity aluminum using the segregation method. This device utilizes the temperature difference between the aluminum liquid and the crystallizer to achieve crystallization and purification effects. The temperature control of the crystallizer will affect the content of impurities in high-purity aluminum. By precisely controlling the temperature of the crystallizer, the purity of aluminum can be improved. Using an instant heating cooling device and adjusting the flow rate of the cooling device without affecting the water temperature control to ensure the cooling effect, thereby precisely controlling the cooling temperature, which is conducive to the segregation and separation of impurity elements. However, because this device needs to precisely adjust the water temperature, frequent water temperature control adjustments will reduce the service life of the equipment and require a relatively high equipment cost. In addition, the instant heating cooling device also increases the demand for water.

[0010] At present, there is no method and equipment in the industry that publicly uses the segregation smelting method to achieve the continuous preparation of refined antimony. Summary of the Invention

[0011] To solve the above problems, the present invention provides a method and equipment for gravity continuous segregation smelting of refined antimony.

[0012] The technical solution of the present invention is realized as follows: A method for gravity continuous segregation smelting of refined antimony includes the following technological steps:

[0013] Step 1: Crush 5000 kg of 95% crude antimony raw materials to a suitable particle size, open the feeding bin cover, lower the graphite gate of the melting bin, put the crude antimony raw materials into the feeding bin, close the feeding bin cover, inject pure water into the product collection pool to the set liquid level, run the inert gas replacement process, and maintain a slightly positive pressure environment;

[0014] Step 2: Raise the temperature of the melting bin to 680 °C, melt all the input crude antimony raw materials into a liquid state, raise the temperature and maintain the lining plate temperature of the first segregation bin, the second segregation bin, and the third segregation bin at 630 °C;

[0015] Step 3: Lower the graphite gates of the extraction areas of the first segregation bin, the second segregation bin, and the third segregation bin respectively, move the condensation plate A of the first segregation bin, the condensation plate C of the second segregation bin, and the condensation plate E of the third segregation bin to the corresponding extraction areas of the segregation bins respectively, move the condensation plate B of the first segregation bin, the condensation plate D of the second segregation bin, and the condensation plate F of the third segregation bin to the corresponding collection areas of the segregation bins respectively, raise the condensation plate A, the condensation plate C, and the condensation plate E to the highest point and introduce circulating cooling water, lower the condensation plate B, the condensation plate D, and the condensation plate F to the lowest point, empty the circulating cooling water in the condensation plate B and then raise its temperature to 650 °C;

[0016] Step 4: Raise the graphite gate of the melting bin, release 1000 kg of liquid antimony in it to the extraction area of the first segregation bin, lower the graphite gate of the melting bin, lower the condensation plate A in the first segregation bin to the lowest point to contact the antimony liquid surface, after running for 1 h, raise the condensation plate A to the highest point and empty the circulating cooling water, raise the condensation plate B in the first segregation bin to the highest point, turn off the heating wire and introduce circulating cooling water, move the condensation plate A in the first segregation bin to the collection area, and move the condensation plate B in the first segregation bin to the extraction area;

[0017] Step 5: Lower the graphite gate of the second segregation bin, raise the graphite gate of the first segregation bin, release the liquid antimony in the extraction area of the first segregation bin to the extraction area of the second segregation bin, lower the graphite gate of the first segregation bin, lower the condensation plate C in the second segregation bin to the lowest point to contact the antimony liquid surface, lower the condensation plate A in the first segregation bin to the lowest point and raise its temperature to 650 °C;

[0018] Step Six: Lift the graphite gate of the chemical storage bin, release 1000 kg of liquid antimony into the extraction area of the first segregation bin, lower the graphite gate of the chemical storage bin, lower the condensation plate B in the first segregation bin to the lowest point to contact the antimony liquid surface, and run for 1 h;

[0019] Step Seven: Lift the condensation plates B and C to the highest point and drain the circulating cooling water, lift the condensation plates A and D to the highest point, turn off the heating wire and introduce the circulating cooling water, move the condensation plates B and C to the collection area, and move the condensation plates A and D to the extraction area;

[0020] Step Eight: Lower the graphite gate of the third segregation bin, lift the graphite gate of the second segregation bin, release the liquid antimony in the extraction area of the second segregation bin into the extraction area of the third segregation bin, lower the graphite gate of the second segregation bin, lift the graphite gate of the first segregation bin, release the liquid antimony in the extraction area of the first segregation bin into the extraction area of the second segregation bin, lower the graphite gate of the first segregation bin, lift the graphite gate of the chemical storage bin, and release 1000 kg of liquid antimony into the extraction area of the first segregation bin;

[0021] Step Nine: Lower the condensation plates A, D, and E to the lowest point to contact the antimony liquid surface, lower the condensation plates B, C, and F to the lowest point and heat them up to 650 °C, and run for 1 h;

[0022] Step Ten: Raise the condensation plates A, D, and E to the highest point and drain the circulating cooling water, raise the condensation plates B, C, and F to the highest point, turn off the heating wire and introduce the circulating cooling water, move the condensation plates A, D, and E to the collection area, move the condensation plates B, C, and F to the extraction area, lift the graphite gate of the third segregation bin, and drain the liquid residual antimony into the tailing collection tank;

[0023] Step Eleven: Lower the graphite gate of the third segregation bin, lift the graphite gate of the second segregation bin, release the liquid antimony in the extraction area of the second segregation bin into the extraction area of the third segregation bin, lower the graphite gate of the second segregation bin, lift the graphite gate of the first segregation bin, release the liquid antimony in the extraction area of the first segregation bin into the extraction area of the second segregation bin, lower the graphite gate of the first segregation bin, lift the graphite gate of the chemical storage bin, and release 1000 kg of liquid antimony into the extraction area of the first segregation bin;

[0024] Step Twelve: Lower the condensation plates B, C, and F to the lowest point to contact the antimony liquid surface, lower the condensation plates A, D, and E to the lowest point and heat them up to 650 °C, and run for 1 h;

[0025] Step Thirteen: Raise Condensation Plates B, C, and F to the highest point and drain the circulating cooling water. Raise Condensation Plates A, D, and E to the highest point, turn off the heating wire, and introduce circulating cooling water. Move Condensation Plates B, C, and F to the collection area, and move Condensation Plates A, D, and E to the extraction area. Lift the graphite gate of the No. 3 segregation bin and discharge the liquid residual antimony into the tailing collection pool.

[0026] Step Fourteen: Repeat Steps Eight to Thirteen twice. Crush 4000 kg of 95% crude antimony raw materials to an appropriate particle size. Open the feed bin cover, put the crude antimony raw materials into the feed bin, close the feed bin cover, run the inert gas replacement process, maintain a slightly positive pressure environment, collect the 99.9% refined antimony products in the product collection pool, dehydrate and dry them, then put them into a melting furnace for melting, ingot casting, sampling, packaging, numbering, weighing, and storage. Collect the residual antimony in the tailing collection pool and properly dispose of it.

[0027] Step Fifteen: Repeat Steps Eight to Fourteen and keep the system running until shutdown.

[0028] An equipment for gravity continuous segregation refining of antimony, including a raw material preparation device, a continuous segregation refining device, an output product collection device, and an auxiliary monitoring device. The raw material preparation device includes a feed bin and a melting bin. The feed bin is installed on a feed bin support seat, and the feed bin is provided with a feed bin cover. The melting bin is installed on a melting bin support column. The material inlet side of the melting bin is connected to the feed bin. The melting bin is provided with a melting bin cover and an observation window. A graphite gate is provided on the material outlet side of the melting bin, and a thermocouple is provided at the bottom of the graphite gate. A graphite lining is provided inside the melting bin, and heating wires are arranged outside the graphite lining.

[0029] Preferably, the continuous segregation smelting device includes a first segregation bin, a second segregation bin, and a third segregation bin. The segregation bins are all installed on segregation bin support seats. The structures of the 3 segregation bins are the same. A segregation bin cover is provided on the segregation bin. Two mutually isolated areas, namely an extraction area and a collection area, are provided inside the segregation bin. The material output sides of the extraction area and the collection area of the first segregation bin are respectively connected to the extraction area and the collection area of the second segregation bin. The material output sides of the extraction area and the collection area of the second segregation bin are respectively connected to the extraction area and the collection area of the third segregation bin. The material output sides of the extraction area and the collection area of the third segregation bin are respectively connected to the product collection pool of the product collection device. Graphite gates are provided on the material outflow sides of the extraction area and the collection area inside each segregation bin. A thermocouple is provided at the bottom end of the graphite gate. A graphite lining is provided inside the segregation bin. Heating wires are arranged outside the graphite lining. Two condensers are provided inside each segregation bin. The mother seats of the condensers are respectively connected to the segregation bin cover through slide rails. Telescopic cylinders are provided below the mother seats of the condensers. The condensation plates on the condensers are connected to the telescopic cylinders. A refrigerant pipeline and an electric heating wire are provided inside the condensation plates. The inlet and return circuits of the refrigerant pipeline and the electric heating wire inside the condensation plates pass through the telescopic cylinders and are connected to the condenser mother seats and the segregation bin cover;

[0030] Preferably, the product collection device includes a product collection pool, a collection pool base, and a pure water control system. The product collection pool is arranged on the collection pool base. Two mutually isolated areas, namely a product collection pool and a tailing collection pool, are provided inside the product collection pool. Pure water is provided inside the product collection pool and the tailing collection pool. A pure water control system is provided on the product collection pool. The pure water control system includes a liquid level detection sensor, a water supply pipeline, and a drainage pipeline;

[0031] Preferably, the auxiliary monitoring device includes a sensor integration module, an inert gas control pipeline, a vacuum pump, and a pressure relief valve. The sensor integration module includes a pressure sensor, a temperature sensor, and a liquid level sensor. The sensor integration module is respectively placed inside the material melting bin and each segregation bin and is connected to the material melting bin cover and the segregation bin cover. The inert gas control pipeline is externally connected to a high-purity inert gas source. The inert gas control pipeline and the vacuum pipeline of the vacuum pump respectively extend into the material melting bin and the segregation bin through the material melting bin cover and each segregation bin cover. The pressure relief valves are respectively installed on the material melting bin cover and each segregation bin cover and communicate with the material melting bin and the segregation bin;

[0032] Preferably, the graphite lining on the bottom surface of the material melting bin has a slope of 8-12°;

[0033] Preferably, the graphite linings on the bottom surfaces of the first segregation bin, the second segregation bin, and the third segregation bin all have a slope of 8-12°;

[0034] Preferably, the heights of the support seats of the material melting bin, the first segregation bin, the second segregation bin, and the third segregation bin decrease by 180-220 mm in sequence;

[0035] Preferably, the refrigerant used in the refrigerant pipeline inside the condensation plate is circulating cooling water;

[0036] Preferably, the vacuum pump is a rotary vane vacuum pump.

[0037] Supplement the principle of the present invention and explain the reason why such a setting can solve the problems of the invention.

[0038] The segregation smelting method is applied to the field of refined antimony smelting, making full use of the difference in the distribution coefficient of impurity elements between the liquid and solid phases during the solidification of metals, so that impurities with an equilibrium distribution coefficient less than 1 are continuously transferred and enriched in the liquid phase and finally enter the tailings. The overall process flow is simple, can operate continuously, and has the advantage of low energy consumption compared with traditional smelting methods.

[0039] The beneficial effects of the present invention are as follows: 1) Compared with the existing antimony metal smelting technology, the present invention utilizes the principle of segregation purification and combines the situation that the distribution coefficients of most impurities in antimony are less than 1 to achieve efficient and continuous smelting of refined antimony under low temperature difference conditions. The process flow is simple, the recovery rate is high, and the waste is less.

[0040] 2) The number of operating segregation bins can be adjusted according to the quality of the raw materials to ensure the product quality, and it has good adaptability to raw materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 is a schematic structural diagram of the equipment of the present invention;

[0042] Figure 2 is a top view of the present invention;

[0043] Part description: 1. Raw material preparation device:

[0044] 101. Feeding bin, 102. Melting bin, 103. Feeding bin support seat, 104. Feeding bin cover, 105. Melting bin support seat, 106. Melting bin cover, 108. Graphite gate of the melting bin, 110. Graphite lining of the melting bin;

[0045] Segregation smelting device:

[0046] The first segregation bin, 2101. Segregation bin support seat, 2102. Extraction area of the first segregation bin, 2103. Collection area of the first segregation bin, 2104. Cover of the first segregation bin, 2105. Observation window, 2106. Graphite gate of the extraction area of the first segregation bin, 2107. Graphite gate of the collection area of the first segregation bin, 2110. Graphite lining of the first segregation bin;

[0047] 2200. Condenser A, 2201. Condenser B, 2204. Slide rail of the first segregation bin, 2205. Telescopic cylinder, 2206. Condensing plate A, 2207. Condensing plate B;

[0048] 2300. Second segregation bin, 2301. Support seat of the second segregation bin, 2302. Extraction area of the second segregation bin, 2303. Collection area of the second segregation bin, 2304. Cover of the second segregation bin, 2306. Graphite gate in the extraction area of the second segregation bin, 2307. Graphite gate in the collection area of the second segregation bin, 2310. Graphite lining of the second segregation bin;

[0049] 2400. Condenser C, 2401. Condenser D, 2404. Slide rail of the second segregation bin, 2405. Telescopic cylinder, 2406. Condensing plate C, 2407. Condensing plate D;

[0050] 2500. Third segregation bin, 2501. Support seat of the third segregation bin, 2502. Extraction area of the third segregation bin, 2503. Collection area of the third segregation bin, 2504. Cover of the third segregation bin, 2506. Graphite gate in the extraction area of the third segregation bin, 2507. Graphite gate in the collection area of the third segregation, 2510. Graphite lining of the third segregation bin;

[0051] 2600. Condenser E, 2601. Condenser F, 2604. Slide rail of the third segregation bin, 2605. Telescopic cylinder, 2606. Condensing plate E, 2607. Condensing plate F;

[0052] 3. Product collection device: 301. Output product collection pool, 302. Base of the product collection pool, 303. Pure water control system, 304. Product collection pool, 305. Tailings collection pool;

[0053] 4. Auxiliary monitoring device: 401. Sensor integration module, 403. Vacuum pump, 404. Pressure regulating valve. Detailed implementation mode

[0054] In order to make the objectives, technical solutions and advantages of the present invention clearer and more understandable, the following further details the present invention in conjunction with embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention. Embodiment

[0055] A method for smelting self-flow continuous segregation refined antimony includes the following technological steps:

[0056] Step 1: Crush 5000 kg of 95% crude antimony raw materials to an appropriate particle size. Open the feeding bin cover 104, lower the graphite gate 108 of the melting bin, put the crude antimony raw materials into the feeding bin 101, close the feeding bin cover 104, inject pure water into the product collection tank 304 to the set liquid level, run the inert gas replacement process, and maintain a slightly positive pressure environment. The inert gas replacement ensures that the main atmosphere in the space of the melting bin and each segregation bin is inert gas, avoiding the problem of product oxidation. The pure water in the product collection tank forms a liquid seal with the third segregation bin to prevent the system from communicating with the atmosphere internally;

[0057] Step 2: Raise the temperature of the melting bin 102 to 680 °C to completely melt the input raw material crude antimony into a liquid state, and raise and maintain the temperature of the lining plates of the first, second, and third segregation bins to 630 °C;

[0058] Step 3: Lower the graphite gates 2106 in the extraction area of the first segregation bin, 2306 in the extraction area of the second segregation bin, and 2506 in the extraction area of the third segregation bin. Move the condensation plates A2206, C2406, and E2606 to the corresponding extraction areas of the segregation bins, and move the condensation plates B2207, D2407, and E2607 to the corresponding collection areas of the segregation bins. Lift the condensation plates A2206, C2406, and E2606 to the highest point and introduce circulating cooling water. Lower the condensation plates B2207, D2407, and E2607 to the lowest point, empty the circulating cooling water in the condensation plate B2207, and then raise its temperature to 650 °C;

[0059] Step 4: Lift the graphite gate 108 of the melting bin, release 1000 kg of liquid antimony into the extraction area 2102 of the first segregation bin, lower the graphite gate 108 of the melting bin, lower the condensation plate A2206 to the lowest point to contact the antimony liquid surface. After running for 1 h, lift the condensation plate A2206 to the highest point and empty the circulating cooling water. Lift the condensation plate B2207 to the highest point, turn off the heating wire and introduce circulating cooling water. Move the condensation plate A2206 to the collection area 2103 of the first segregation bin, and move the condensation plate B2207 to the extraction area 2102 of the first segregation bin;

[0060] Step 5: Lower the graphite gates 2306 and 2307 of the second segregation bin, lift the graphite gates 2106 and 2107 of the first segregation bin, release the liquid antimony in the extraction area 2102 of the first segregation bin into the extraction area 2302 of the second segregation bin, lower the graphite gates 2106 and 2107 of the first segregation bin, lower the condensation plate C2406 to the lowest point to contact the antimony liquid surface, and lower the condensation plate A2206 to the lowest point and raise its temperature to 650 °C;

[0061] Step 6: Lift the graphite gate 108 of the chemical feeding bin, release 1000 kg of liquid antimony into the extraction area 2102 of the first segregation bin, lower the graphite gate 108 of the chemical feeding bin, lower the condensation plate B2207 to the lowest point to contact the antimony liquid surface, and after operating for 1 h;

[0062] Step 7: Lift the condensation plate B2207 and the condensation plate C2406 to the highest point and drain the circulating cooling water. Lift the condensation plate A2206 and the condensation plate D2407 to the highest point, turn off the heating wire and introduce the circulating cooling water. Move the condensation plate B2207 and the condensation plate C2406 to the collection area, and move the first condensation plate A2206 and the condensation plate D2407 to the extraction area;

[0063] Step 8: Lower the graphite gates 2506 and 2507 of the third segregation bin, lift the graphite gates 2306 and 2307 of the second segregation bin, release the liquid antimony in the extraction area 2302 of the second segregation bin into the extraction area 2502 of the third segregation bin, lower the graphite gates 2306 and 2307 of the second segregation bin, lift the graphite gates 2106 and 2107 of the first segregation bin, release the liquid antimony in the extraction area 2102 of the first segregation bin into the extraction area 2302 of the second segregation bin, lower the graphite gates 2106 and 2107 of the first segregation bin, lift the graphite gate 108 of the chemical feeding bin, and release 1000 kg of liquid antimony into the extraction area 2102 of the first segregation bin;

[0064] Step 9: Lower the condensation plate A2206, the condensation plate D2407, and the condensation plate E2606 to the lowest point to contact the antimony liquid surface. Lower the condensation plate B2207, the condensation plate C2406, and the condensation plate F2607 to the lowest point and heat them up to 650 °C, and operate for 1 h;

[0065] Step 10: Raise the condensation plate A2206, the condensation plate D2407, and the condensation plate E2606 to the highest point and drain the circulating cooling water. Raise the condensation plate B2207, the condensation plate C2406, and the condensation plate F2607 to the highest point, turn off the heating wire and introduce the circulating cooling water. Move the condensation plate A2206, the condensation plate D2407, and the condensation plate E2606 to the collection area, move the condensation plate B2207, the condensation plate C2406, and the condensation plate F2607 to the extraction area, and lift the graphite gates 2506 and 2507 of the third segregation bin to discharge the liquid residual antimony into the tailing collection pool 305;

[0066] Step 11: Lower the graphite gates 2506 and 2507 of the third segregation bin, raise the graphite gates 2306 and 2307 of the second segregation bin, discharge the liquid antimony in the extraction area 2302 of the second segregation bin into the extraction area 2502 of the third segregation bin, lower the graphite gates 2306 and 2307 of the second segregation bin, raise the graphite gates 2106 and 2107 of the first segregation bin, discharge the liquid antimony in the extraction area 2102 of the first segregation bin into the extraction area 2302 of the second segregation bin, lower the graphite gates 2106 and 2107 of the first segregation bin, raise the graphite gate 108 of the charging bin, and discharge 1000 kg of liquid antimony into the extraction area 2102 of the first segregation bin;

[0067] Step 12: Lower the condensation plates B2207, C2406, and F2607 to the lowest point to contact the antimony liquid surface, lower the condensation plates A2206, D2407, and E2606 to the lowest point and heat them up to 650 °C, and run for 1 h;

[0068] Step 13: Raise the condensation plates B2207, C2406, and F2607 to the highest point and drain the circulating cooling water, raise the condensation plates A2206, D2407, and E2606 to the highest point, turn off the heating wire and introduce circulating cooling water, move the condensation plates B2207, C2406, and F2607 to the collection area, move the condensation plates A2206, D2407, and E2606 to the extraction area, and raise the graphite gates 2506 and 2507 of the third segregation bin to discharge the liquid residual antimony into the tailing collection tank 304;

[0069] Step 14: Repeat Steps 8 to 13 twice, crush 4000 kg of 95% crude antimony raw materials to appropriate particle sizes, open the charging bin cover 104, put the crude antimony raw materials into the charging bin 101, close the charging bin cover 104, run the inert gas replacement process, maintain a slightly positive pressure environment, collect the 99.5% refined antimony products in the product collection tank, dehydrate and dry them, put them into the melting furnace for melting, casting, sampling, packaging, numbering, weighing, and storage, collect the residual antimony in the tailing collection tank and properly dispose of it;

[0070] Step 15: Repeat Steps 8 to 14 and keep the system running until shutdown.

[0071] An equipment for continuous gravity segregation refining of antimony includes a raw material preparation device 1, which is used to provide liquid crude antimony raw materials for smelting production. The raw material preparation device 1 includes a feeding bin 101, a feeding bin support seat 103, a feeding bin cover 104, a material melting bin 102, a material melting bin support seat 105, a material melting bin cover 106, a graphite gate 108 for the material melting bin, a thermocouple, a graphite lining plate 110, and a heating wire 1. The feeding bin 101 is installed on the feeding bin support seat 103 and stands on the ground. A feeding bin cover 104 is installed on the feeding bin 101, and the inner bottom surface of the feeding bin 101 has a 10° slope. The material melting bin 102 is installed on the material melting bin support seat 105 and stands on the ground. The material inlet side of the material melting bin 102 is connected to the feeding bin 101. A material melting bin cover 106 is installed on the material melting bin 102 and is provided with an observation window. A graphite gate 108 for the material melting bin is provided on the material outlet side of the material melting bin 102. A thermocouple is installed at the bottom end of the graphite gate 108 for the material melting bin. The inside of the material melting bin is lined with a high-temperature graphite lining plate 110. The graphite lining plate 110 on the bottom surface of the material melting bin 102 has a 10° slope. Heating wires are arranged outside the graphite lining plate 110 of the material melting bin.

[0072] The continuous segregation smelting device 2 includes a first segregation bin 2100, a condenser A 2200, a condenser B 2201, a second segregation bin 2300, a condenser C 2400, a condenser D 2401, a third segregation bin 2500, a condenser E 2600, and a condenser F 2601. The first segregation bin 2100 is installed on a first segregation bin support base 2101 and stands on the ground. The interior of the first segregation bin 2100 is divided into two mutually isolated areas, an extraction area 2102 and a collection area 2103. The material inlet side of the extraction area 2102 of the first segregation bin is connected to the material melting bin 102. The material output sides of the extraction area 2102 and the collection area 2103 of the first segregation bin are respectively connected to the extraction area 2302 and the collection area 2303 of the second segregation bin 2300. The first segregation bin 2100 is equipped with a first segregation bin cover 2104 and is provided with an observation window. At the material outflow sides of the extraction area 2102 and the collection area 2103 inside the first segregation bin 2100, there are respectively a first segregation bin graphite gate 2106 and 2107. Thermocouples are installed at the bottoms of the first segregation bin graphite gates 2106 and 2107. The interior of the first segregation bin 2100 is lined with high-purity graphite lining 2110. The graphite lining 2110 on the bottom surface of the first segregation bin has a 10° slope. Heating wires are arranged outside the graphite lining 2110 of the first segregation bin. The condenser A 2200 and the condenser B 2201 each consist of two identical parts. The two mother seats of the condenser A 2200 and the condenser B 2201 are respectively connected to the first segregation bin cover 2104 through slide rails 2204. Four telescopic columns 2205 are connected below the mother seats. The condensation plate A 2206 of the condenser A 2200 and the condensation plate B 2207 of the condenser B 2201 are connected to the telescopic columns 2205. Refrigerant pipelines and electric heating wires are provided inside the condensation plate A 2206 and the condensation plate B 2207. The inlets and circuits of the refrigerant pipelines and the electric heating wires are connected to the mother seats through the telescopic columns 2205 and then to the first segregation bin cover 2104. The second segregation bin 2300 is installed on a second segregation bin support base 2301 and stands on the ground. The interior of the second segregation bin 2300 is divided into two mutually isolated areas, an extraction area 2302 and a collection area 2303. The material inlet sides of the extraction area 2302 and the collection area 2303 of the second segregation bin are respectively connected to the extraction area 2102 and the collection area 2103 of the first segregation bin. The material output sides of the extraction area 2302 and the collection area 2303 of the second segregation bin are respectively connected to the extraction area 2502 and the collection area 2503 of the third segregation bin 2500. The second segregation bin 2300 is equipped with a second segregation bin cover 2304 and is provided with an observation window. At the material outflow sides of the extraction area 2302 and the collection area 2303 inside the second segregation bin, there are respectively a second segregation bin graphite gate 2306 and 2307. Thermocouples are installed at the bottoms of the second segregation bin graphite gates 2306 and 2307. The interior of the second segregation bin 2300 is lined with high-purity graphite lining 2310. The graphite lining 2310 on the bottom surface of the second segregation bin 2300 has a 10° slope.A heating wire is arranged outside the graphite lining plate 2310 of the No. 2 segregation bin. The condensers C2400 and D2401 include two identical parts. The two mother seats of the condensers C2400 and D2401 are respectively connected to the No. 2 segregation bin cover 2304 through slide rails 2404. Four telescopic cylinders 2405 are connected below the mother seats of the condensers C2400 and D2401. The condenser plates C2406 and D2407 are connected to the telescopic cylinders 2405. Refrigerant pipelines and electric heating wires are arranged inside the condenser plates C2406 and D2407. The inlets and return circuits of the refrigerant pipelines and the electric heating wires are connected to the No. 2 segregation bin cover 2304 through the telescopic cylinders 2405 and the mother seats. The No. 3 segregation bin 2500 is installed on the No. 3 segregation bin support seat 2501 and stands on the ground. The interior of the No. 3 segregation bin is divided into two mutually isolated areas, namely an extraction area 2502 and a collection area 2503. The material inlet sides of the extraction area 2502 and the collection area 2503 of the No. 3 segregation bin are respectively connected to the extraction area 2302 and the collection area 2303 of the No. 2 segregation bin. The material outlet sides of the extraction area 2502 and the collection area 2503 of the No. 3 segregation bin are respectively connected to the tail material collection pool 305 and the product collection pool 304 of the product collection device 3. The No. 3 segregation bin 2500 is equipped with a No. 3 segregation bin cover 2504 and is provided with an observation window. Graphite gates 2506 and 2507 of the No. 3 segregation bin are respectively arranged on the material outflow sides of the extraction area 2502 and the collection area 2503 in the No. 3 segregation bin. Thermocouples are respectively installed at the bottoms of the graphite gates 2506 and 2507 of the No. 3 segregation bin. The interior of the No. 3 segregation bin 2500 is a high-purity graphite lining plate 2510. The graphite lining plate 2510 at the bottom of the No. 3 segregation bin 2500 has a slope of 10°. A heating wire is arranged outside the graphite lining plate 2510 of the No. 3 segregation bin. The condensers E2600 and F2601 include two identical parts. The two mother seats of the condensers E2600 and F2601 are respectively connected to the No. 3 segregation bin cover 2504 through slide rails 2604. Four telescopic cylinders 2605 are connected below the mother seats of the condensers E2600 and F2601. The condenser plates E2606 and F2607 are connected to the telescopic cylinders 2605. Refrigerant pipelines and electric heating wires are arranged inside the condenser plates E2606 and F2607. The inlets and return circuits of the refrigerant pipelines and the electric heating wires are connected to the No. 3 segregation bin cover 2504 through the telescopic cylinders 2605 and the mother seats. The heights of the support seats of the material melting bin 102, the No. 1 segregation bin 2100, the No. 2 segregation bin 2300, and the No. 3 segregation bin 2500 decrease by 200 mm in sequence.,

[0073] The product collection device 3 is used to collect and cool refined antimony products and tailing residual antimony during the production process, and includes a product output collection pool 301, a collection pool base 302, and a pure water control system 303. The product output collection pool 301 is installed on the collection pool base 302. The interior of the product output collection pool 301 is divided into two mutually isolated areas, namely a product collection pool 304 and a tailing collection pool 305. The material inlet sides of the product collection pool 304 and the tailing collection pool 305 are respectively connected to the collection area 2503 and the extraction area 2502 of the third segregation bin 2500. The product collection pool 304 and the tailing collection pool 305 are filled with pure water. The pure water control system 303 includes a liquid level detection sensor, a water replenishing pipeline, and a drainage pipeline. The pure water control system 303 can monitor the pure water liquid level in the product collection pool 304 and the tailing collection pool 305 in real time, and realize the functions of automatic water replenishment and water replacement.

[0074] The auxiliary monitoring device 4 is used to monitor the internal pressure, temperature, and liquid level of the system during the production process, and control the inert gas replacement and pressure relief of the system. It includes a sensor integration module 401, an inert gas control pipeline, a vacuum pump 403, and a pressure relief valve 404. The sensor integration module 401 includes a pressure sensor, a temperature sensor, and a liquid level sensor. The sensor integration module 401 is respectively placed in the material melting bin 102, the first segregation bin 2100, the second segregation bin 2300, and the third segregation bin 2500 and is connected to the material melting bin cover 106, the first segregation bin cover 2104, the second segregation bin cover 2304, and the third segregation bin cover 2504. The inert gas control pipeline is externally connected to a high-purity inert gas source. The inert gas control pipeline extends into the material melting bin 102, the first segregation bin 2100, the second segregation bin 2300, and the third segregation bin 2500 respectively through the material melting bin cover 106, the first segregation bin cover 2104, the second segregation bin cover 2304, and the third segregation bin cover 2504. The vacuum pipeline of the vacuum pump 403 extends into the material melting bin 102, the first segregation bin 2100, the second segregation bin 2300, and the third segregation bin 2500 respectively through the material melting bin cover 106, the first segregation bin cover 2104, the second segregation bin cover 2304, and the third segregation bin cover 2504. The pressure relief valve 404 is respectively installed on the material melting bin cover 106, the first segregation bin cover 2104, the second segregation bin cover 2304, and the third segregation bin cover 2504 and communicates with the material melting bin 102, the first segregation bin 2100, the second segregation bin 2300, and the third segregation bin 2500.

[0075] In the current national standard of the People's Republic of China GB / T 1599-2014, antimony ingots are classified into four grades according to chemical composition: Sb99.50, Sb99.65, Sb99.70, and Sb99.90.

[0076] The following table is a comparison table of the requirements for the contents of main impurity elements listed in the Sb99.50 grade of the current National Standard of the People's Republic of China GB / T 1599-2014 and the test results of the raw material 95% crude antimony and the product 99.5% refined antimony in Example 1. Both the raw material and the product were tested by inductively coupled plasma-mass spectrometry (ICP-MS) (unit: %).

[0077] Judging from the test results, through the continuous segregation refining method and equipment for refined antimony with self-flow described in the present invention, it is possible to use 95% crude antimony as the raw material and prepare 99.5% refined antimony through continuous segregation purification.

[0078]

[0079] The above content is a further detailed description of the present invention in combination with specific preferred embodiments. It cannot be determined that the specific implementation of the present invention is only limited to these descriptions. For those of ordinary skill in the technical field to which the present invention pertains, without departing from the concept of the present invention, several simple deductions or substitutions can still be made, and all should be regarded as belonging to the protection scope of the present invention.

Claims

1. A device for self-flowing continuous segregation refined antimony smelting, characterized in that The invention comprises a raw material preparation device (1), a continuous segregation smelting device (2), an output product collection device (3), and an auxiliary monitoring device (4). The raw material preparation device (1) comprises a feeding bin (101) and a chemical bin (102). The feeding bin (101) is mounted on a feeding bin support seat (103). The feeding bin (101) is provided with a feeding bin cover (104). The chemical bin (102) is mounted on a chemical bin support column (105). The material inlet side of the chemical bin (102) is connected to the feeding bin (101). The chemical bin (102) is provided with a chemical bin cover (106) and an observation window. A graphite gate (108) is provided on the material outflow side of the chemical bin (102). A thermocouple is provided at the bottom of the graphite gate (108). A graphite lining plate (110) is provided inside the chemical bin (102). A heating wire is arranged outside the graphite lining plate (110). The continuous segregation smelting device (2) comprises a No. 1 segregation bin (2100), a No. 2 segregation bin (2300), and a No. 3 segregation bin (2500), wherein the segregation bins are all mounted on segregation bin support seats, and the three segregation bins have the same structure. A segregation bin cover is provided on the segregation bin, and two mutually isolated areas, an extraction area and a collection area, are provided in the segregation bins. The material outflow side of the chemical bin (102) is connected to the No. 1 segregation bin extraction area (2102), and the material output sides of the No. 1 segregation bin extraction area (2102) and the collection area (2103) are respectively connected to the No. 2 segregation bin extraction area (2302) and the collection area (2303), and the material output sides of the No. 2 segregation bin extraction area (2302) and the collection area (2303) are respectively connected to the No. 3 segregation bin extraction area (2502) and the collection area (2503). ), the material output sides of the extraction area (2502) and the collection area (2503) of the third segregation bin are respectively connected to the product collection pool (304) and the tailings collection pool (305) of the output product collection device (3), and graphite gates are provided on the material outflow sides of the extraction area and the collection area in each segregation bin, and a thermocouple is provided at the bottom of the graphite gate. A graphite lining is provided inside the segregation bin, and a heating wire is arranged outside the graphite lining. Two condensers are provided in each segregation bin, and the mother seats of the condensers are connected to the segregation bin cover through slide rails. A telescopic column is provided under the mother seat of the condenser, and a condensation plate on the condenser is connected to the telescopic column. A refrigerant pipeline and an electric heating wire are provided in the condensation plate, and the refrigerant pipeline and the electric heating wire in the condensation plate are connected to the segregation bin cover through the telescopic column.

2. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1, characterized in that The output product collection device (3) comprises an output product collection pool (301), a collection pool base (302), and a pure water control system (303); the output product collection pool (301) is arranged on the collection pool base (302); two mutually isolated areas, namely a product collection pool (304) and a tailings collection pool (305) are arranged in the output product collection pool (301); pure water is arranged in the product collection pool (304) and the tailings collection pool (305); a pure water control system (303) is arranged on the output product collection pool (301); and the pure water control system (303) comprises a liquid level detection sensor, a water supply pipeline, and a drainage pipeline.

3. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1, characterized in that The auxiliary monitoring device (4) comprises a sensor integrated module (401), an inert gas control pipeline, a vacuum pump (403), and a pressure relief valve (404). The sensor integrated module (401) comprises a pressure sensor, a temperature sensor, and a liquid level sensor. The sensor integrated modules (401) are respectively placed in the chemical bin (102) and each segregation bin and connected to the chemical bin cover and the segregation bin cover. The inert gas control pipeline is externally connected to a high-purity inert gas source. The inert gas control pipeline and the vacuum pipeline of the vacuum pump (403) extend into the chemical bin and the segregation bin through the chemical bin cover and each segregation bin cover respectively. The pressure relief valve (404) is respectively installed on the chemical bin cover and each segregation bin cover and connects the chemical bin and the segregation bin.

4. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1, characterized in that The graphite lining plate (110) of the chemical storage bin (102) at the bottom surface is provided with a slope of 8 to 12 degrees.

5. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1, characterized in that The graphite lining plates on the bottom surfaces of the No. 1 segregation bin (2100), the No. 2 segregation bin (2300) and the No. 3 segregation bin (2500) are all provided with a slope of 8 to 12 degrees.

6. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1 or 5, characterized in that The heights of the support seats of the chemical bin (102), the first segregation bin (2100), the second segregation bin (2300), and the third segregation bin (2500) are sequentially reduced by 180-220 mm.

7. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 1, characterized in that The refrigerant used in the refrigerant pipeline inside the condensing plate is circulating cooling water.

8. The device for self-flowing continuous segregation refined antimony smelting as claimed in claim 3, characterized in that The vacuum pump (403) is a rotary vane vacuum pump.

9. A method for using the self-flowing continuous segregation concentrated antimony smelting equipment according to any one of claims 1 to 8, characterized in that it comprises the following process steps: Step 1: crush 5000 kg of 95% crude antimony raw material to a suitable particle size, open the feeding bin cover (104), drop the graphite gate (108) of the feeding bin, put the crude antimony raw material into the feeding bin (101), close the feeding bin cover (104), inject pure water into the product collection pool (304) to the set liquid level, run the inert gas replacement process, and maintain a slightly positive pressure environment; Step 2: raising the temperature of the heating silo (102) to 680°C, melting all the raw material crude antimony that has been put into liquid, raising the temperature and maintaining the temperature of the graphite lining plates of the No. 1 segregation silo (2100°C), the No. 2 segregation silo (2300°C), and the No. 3 segregation silo (2500°C) to 630°C; Step 3: Lower the graphite gates (2106), (2306), (2506) of the extraction areas of the No. 1 segregation chamber, the No. 2 segregation chamber, and the No. 3 segregation chamber respectively, move the condensation plate A (2206) of the No. 1 segregation chamber, the condensation plate C (2406) of the No. 2 segregation chamber, and the condensation plate E (2606) of the No. 3 segregation chamber to the extraction areas of the corresponding segregation chambers, and move the condensation plate B (2207) of the No. 1 segregation chamber, the condensation plate D (2208) of the No. 2 segregation chamber to the extraction areas of the corresponding segregation chambers. 2407), and the condensation plate F (2607) of the third segregation bin are moved to the corresponding segregation bin collection area respectively, and the condensation plates A (2206), C (2406), and E (2606) are lifted to the high point and circulating cooling water is introduced, and the condensation plates B (2207), D (2407), and F (2607) are lowered to the low point, and the circulating cooling water of the condensation plate B (2207) is emptied and then heated to 650°C; Step 4: lift the graphite gate (108) of the chemical silo, put 1000kg of liquid antimony therein into the extraction area (2102) of the No. 1 segregation silo, drop the graphite gate (108) of the chemical silo, lower the condensation plate A (2206) in the No. 1 segregation silo to the lowest point to contact the antimony liquid surface, run for 1 hour, lift the condensation plate A (2206) to the highest point and drain the circulating cooling water, lift the condensation plate B (2207) in the No. 1 segregation silo to the highest point, turn off the electric heating wire and introduce circulating cooling water, move the condensation plate A (2206) in the No. 1 segregation silo to the collection area (2103) of the No. 1 segregation silo, and move the condensation plate B (2207) in the No. 1 segregation silo to the extraction area (2102) of the No. 1 segregation silo; Step 5: lower the two graphite gates (2306) and (2307) of the No. 2 segregation chamber, raise the two graphite gates (2106) and (2107) of the No. 1 segregation chamber, release the liquid antimony in the extraction area (2102) of the No. 1 segregation chamber into the extraction area (2302) of the No. 2 segregation chamber, lower the two graphite gates (2106) and (2107) of the No. 1 segregation chamber, lower the condensation plate C (2406) in the No. 2 segregation chamber to the lowest point to contact the antimony liquid surface, lower the condensation plate A (2206) in the No. 1 segregation chamber to the lowest point and heat it to 650°C; Step 6: Lift the graphite gate (108) of the chemical silo, put 1000 kg of liquid antimony into the extraction area (2102) of the No. 1 segregation silo, drop the graphite gate (108) of the chemical silo, lower the condensation plate B (2207) in the No. 1 segregation silo to the lowest point to contact the antimony liquid surface, and run for 1 hour; Step 7: lift the condensation plate B (2207) and condensation plate C (2406) to the highest point and drain the circulating cooling water, lift the condensation plate A (2206) and condensation plate D (2407) to the highest point, turn off the electric heating wire and introduce the circulating cooling water, move the condensation plate B (2207) and condensation plate C (2406) to the collection area of ​​the No. 1 segregation bin and the No. 2 segregation bin respectively, and move the condensation plate A (2206) and condensation plate D (2407) to the extraction area of ​​the No. 1 segregation bin and the No. 2 segregation bin respectively; Step 8: lower the two graphite gates (2506) and (2507) of the No. 3 segregation bin, raise the two graphite gates (2306) and (2307) of the No. 2 segregation bin, and place the liquid antimony in the extraction area (2302) of the No. 2 segregation bin to the extraction area (2502) of the No. 3 segregation bin; lower the two graphite gates (2306) and (2307) of the No. 2 segregation bin, raise the two graphite gates (2106) and (2107) of the No. 1 segregation bin, and place the liquid antimony in the extraction area (2102) of the No. 1 segregation bin to the extraction area (2302) of the No. 2 segregation bin; lower the two graphite gates (2106) and (2107) of the No. 1 segregation bin, raise the graphite gate (108) of the chemical bin, and place 1000 kg of liquid antimony in the extraction area (2102) of the No. 1 segregation bin; Step 9: lower the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to a low point to contact the antimony liquid surface, lower the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to a low point and heat them up to 650°C, and run for 1 hour; Step 10: Raise the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to the highest point and drain the circulating cooling water; raise the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to the highest point, turn off the electric heating wire, and introduce circulating cooling water; move the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to the collection area of ​​the No. 1 segregation bin, the No. 2 segregation bin, and the No. 3 segregation bin respectively; move the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to the extraction area of ​​the No. 1 segregation bin, the No. 2 segregation bin, and the No. 3 segregation bin respectively; raise the two graphite gates (2506) and (2507) of the No. 3 segregation bin to discharge the liquid residual antimony into the tailings collection pool (305); Step 11: lower the two graphite gates (2506) and (2507) of the No. 3 segregation bin, raise the two graphite gates (2306) and (2307) of the No. 2 segregation bin, and place the liquid antimony in the extraction area (2302) of the No. 2 segregation bin to the extraction area (2502) of the No. 3 segregation bin; lower the two graphite gates (2306) and (2307) of the No. 2 segregation bin, raise the two graphite gates (2106) and (2107) of the No. 1 segregation bin, and place the liquid antimony in the extraction area (2102) of the No. 1 segregation bin to the extraction area (2302) of the No. 2 segregation bin; lower the two graphite gates (2106) and (2107) of the No. 1 segregation bin, raise the graphite gate (108) of the chemical bin, and place 1000 kg of liquid antimony in the extraction area (2102) of the No. 1 segregation bin; Step 12: lower the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to a low point to contact the antimony liquid surface, lower the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to a low point and heat them up to 650°C, and run for 1 hour; Step 13: Raise the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to the highest point and drain the circulating cooling water; raise the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to the highest point, turn off the electric heating wire, and introduce circulating cooling water; move the condensation plate B (2207), condensation plate C (2406), and condensation plate F (2607) to the collection area of ​​the No. 1 segregation bin, the No. 2 segregation bin, and the No. 3 segregation bin respectively; move the condensation plate A (2206), condensation plate D (2407), and condensation plate E (2606) to the extraction area of ​​the No. 1 segregation bin, the No. 2 segregation bin, and the No. 3 segregation bin respectively; lift the two graphite gates (2506) and (2507) of the No. 3 segregation bin to discharge the liquid residual antimony into the tailings collection pool (305); Step 14: repeat steps 8 to 13 twice, crush 4000 kg of 95% crude antimony raw material to a suitable particle size, open the feeding bin cover (104), put the crude antimony raw material into the feeding bin (101), close the feeding bin cover (104), run the inert gas replacement process, maintain a slightly positive pressure environment, collect the 99.5% refined antimony product in the product collection pool, dry it after dehydration, put it into the material furnace for melting and casting, sample and package it, number it, weigh it and store it, collect the residual antimony in the tailings collection pool and properly dispose of it; Step 15: Repeat steps 8 to 14, keeping the system running until it stops.

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