Antimony concentrate desiliconization and aluminum pretreatment equipment and sib2o3 preparation process

Abstract

The present application relates to a kind of antimony concentrate desilication aluminum pretreatment equipment and antimony trioxide preparation process, belong to antimony trioxide preparation technical field, the pretreatment equipment provided by the present application includes reaction kettle, vibrating screen and cooling mechanism, cooling mechanism has the rotary cooling cylinder of built-in multi-prong rod, can be while cooling material to it carry out crushing, the present application also provides a kind of antimony trioxide preparation process, including by preceding equipment melt salt preparation, antimony concentrate complex desilication aluminum, mixture cooling crushing and vibrating screen classification grading, then using segmented temperature control antimony white furnace with cofferdam and fire wall is carried out oxidation preparation, finally product detection and melt salt recycling and other steps, the cooling and crushing function of the present application are integrated, simplify the process of desilication aluminum pretreatment, avoid the secondary pollution of material, while through the antimony white furnace of segmented temperature control improves oxidation reaction efficiency, effectively improve the purity and yield of antimony trioxide.

Description

Technical Field

[0001] This invention belongs to the field of antimony trioxide preparation technology, and relates to a pretreatment equipment for desilication and aluminization of antimony concentrate and a process for preparing antimony trioxide. Background Technology

[0002] Antimony, as an important strategic mineral, has a wide range of applications in flame retardants, alloy manufacturing, semiconductor and electronics industries, photovoltaic glass, and other fields. More than 60% of antimony worldwide is used to produce flame retardants, and 20% is used to manufacture alloys. With the rapid development of emerging industries, the purity requirements for antimony products are constantly increasing, especially for antimony trioxide, whose purity directly affects the performance of downstream products.

[0003] Currently, the main raw material for the industrial production of antimony trioxide is antimony concentrate. However, antimony concentrate typically contains impurities such as silicon and aluminum. These impurities severely affect the quality of antimony trioxide, causing the product to fail to meet standards for specific gravity, particle size, and other indicators. They also reduce the efficiency of subsequent oxidation reactions and increase production costs. Therefore, the desilication and aluminization pretreatment of antimony concentrate is a crucial step in the preparation of antimony trioxide.

[0004] Existing desiliconization and aluminization pretreatment technologies for antimony concentrate mainly involve chemical desiliconization and aluminization methods such as acid leaching and alkali leaching. These methods generate a large amount of wastewater during the process. In addition, cooling and crushing must be carried out separately, which is not only cumbersome and inefficient, but also leads to secondary pollution of the materials, further affecting the pretreatment effect.

[0005] In the process of preparing antimony trioxide, most existing antimony white furnaces are single-zone heating systems, which cannot achieve segmented temperature control. This results in the inability to carry out the preheating, oxidation, and heat preservation processes of the material simultaneously, leading to low reaction efficiency. Summary of the Invention

[0006] In view of this, in order to solve the above problems, the present invention provides a pretreatment equipment for desilication and a process for preparing antimony trioxide from antimony concentrate.

[0007] To achieve the above objectives, the present invention provides the following technical solution: a pretreatment device for desiliconization and aluminization of antimony concentrate, comprising a reaction vessel and a vibrating screen, wherein the reaction vessel comprises a cylinder, a jacket is fixedly fitted on the outer wall of the cylinder, a motor I is fixedly fitted on the top of the cylinder, a stirring shaft is rotatably fitted through the top of the cylinder, a feed pipe I is fixedly fitted through the top of the cylinder, and a cover plate is detachably fitted on the top of the feed pipe I; It also includes a cooling mechanism, which includes a frame. Guide plate I and guide plate II are fixed at both ends of the frame, respectively. Guide plate I corresponds to the discharge port at the bottom of the reactor, and guide plate II corresponds to the feed port of the vibrating screen. A cooling cylinder rotates inside the frame to cool the material. The cooling cylinder is equipped with multiple multi-faceted bars. When the cooling cylinder rotates, the multi-faceted bars crush the cooled material.

[0008] Furthermore, the bottom end of the stirring shaft is fixed and has spiral blades wound around it. The spiral blades are used to lift the material in the middle upward. A spiral strip is fixed on the outside of the stirring shaft. The outside of the spiral strip contacts the inner wall of the cylinder and pushes the material at the edge downward during the rotation.

[0009] Furthermore, the cooling cylinder includes two sets of support rods, with the same inner cylinder fixedly mounted on the outer side of both sets of support rods. Support rings are fixedly mounted on the outer walls of both ends of the inner cylinder, and multiple connecting rods are fixedly mounted between the two support rings. The multiple connecting rods are used to support the outer cylinder, and the outer cylinder is fixedly sleeved on the outer wall of the multiple connecting rods, forming a space for accommodating the cooling medium between the outer cylinder and the inner cylinder. A rotating ring is rotatably mounted on the outer wall of the support ring, and the rotating ring is rotatably connected to the outer cylinder. The two rotating rings are respectively connected to the inlet pipe and the outlet pipe.

[0010] Furthermore, a rotating shaft III is rotatably provided on the top of the frame, and two sets of support rods are respectively fixed to the outer walls of both ends of the rotating shaft III. A motor II is fixed on the top of one side of the frame, and the motor II is connected to the rotating shaft III through a sprocket and a chain.

[0011] Furthermore, the inner wall of the inner cylinder is fixedly provided with multiple sets of baffles II, which drive the multi-faceted rod to flip.

[0012] A process for preparing antimony trioxide includes the following steps: S1. The raw materials are processed using the aforementioned antimony concentrate desiliconization and aluminization pretreatment equipment: S1.1 Preparation of molten salt: Weigh industrial molten salt according to the ratio of sodium nitrate to potassium chloride = 1:1, add it to the reaction vessel, add 5% quicklime, heat to 350℃ to melt and stir to activate for 10 minutes; S1.2 Antimony concentrate complexation and desilication of aluminum: Add antimony concentrate in batches into the reactor according to the ratio of molten salt: antimony concentrate = 3:1, heat to 380℃ and stir for 40 minutes, then cool to below 100℃; S1.3 Cooling and Crushing of the Mixture: The mixture prepared in S1.2 is placed in a cooling mechanism for cooling and crushing; S1.4, Vibrating screening and classification: pour the cooled material onto a vibrating screen, which comprises two layers of vibrating meshes (the upper layer is 2 mm, and the lower layer is 0.5 mm), collect the desiliconized aluminum-antimony concentrate below 0.5 mm from the lower layer, return the coarse particles on the upper layer to the reaction kettle for secondary treatment, and sell the middle-layer aluminum-silicon complex salt as a building auxiliary material; S2, starting an antimony white furnace, feeding according to the ratio of desiliconized aluminum-antimony concentrate: refined antimony lumps = 1:3, controlling temperature in sections (preheating at 650°C, oxidizing at 720°C, holding at 780°C), blowing in preheated air to oxidize and volatilize antimony liquid, and subjecting flue gas to quenching, cyclone classification and bag dust collection to obtain antimony trioxide powder; S3, Product detection: measuring the specific gravity of the product with a hydrometer (≥5.1 g / cm 3 is qualified), and measuring the particle size with a 2 μm standard sieve (screen underflow ≥ 98% is qualified); S4, Molten salt recycling: recover molten salt from the antimony white furnace, screen after cooling, supplement 5% of fresh molten salt, and reuse for antimony concentrate pretreatment.

[0013] Further, the antimony white furnace comprises a burner fixedly penetrating through one side of the antimony white furnace, an exhaust pipe fixedly penetrating through the top of the antimony white furnace, a feeding pipe II fixedly penetrating through the top of the antimony white furnace, and two hoppers communicated with the top of the feeding pipe II; The antimony white furnace further comprises a first cofferdam and a second cofferdam fixed to the bottom wall of the antimony white furnace, a first trough formed in the second cofferdam, a second trough formed between the second cofferdam and the first cofferdam, a third trough formed between the first cofferdam and the antimony white furnace, and the burner extends into the third trough; The antimony white furnace further comprises a fire wall arranged inside the antimony white furnace, which is used for cutting off the airflow below a gap between the first trough and the second trough and a gap between the second trough and the third trough, so as to avoid hot airflow channeling.

[0014] Further, the fire wall comprises two sets of first rotating shafts fixed to the top of the antimony white furnace, a first baffle is rotatably sleeved at the bottom end of each first rotating shaft, and heights of the two sets of first baffles are respectively adapted to the first cofferdam and the second cofferdam.

[0015] Further, a material guide assembly is arranged in the first feeding pipe and the second feeding pipe, the material guide assembly comprises a second rotating shaft, an inclined turning plate is rotatably sleeved on the outer wall of the second rotating shaft, and when materials on one side of the turning plate accumulate to a certain weight, the turning plate is naturally pushed open.

[0016] Further, a counterweight is fixedly arranged at the bottom of one side of the turning plate, and after the turning plate turns over and the materials fall, the turning plate can be reset and turned over under the gravity of the counterweight.

[0017] Beneficial effects of the present invention are: 1. The antimony concentrate desiliconization and aluminization pretreatment equipment disclosed in this invention achieves dual functions of cooling and crushing through the cooling cylinder of the cooling mechanism, eliminating the need for separate cooling and crushing equipment, simplifying the process flow, improving pretreatment efficiency, and avoiding secondary pollution of materials during transportation, thus ensuring the purity of the desiliconized and aluminized antimony concentrate. 2. The antimony concentrate desilication and aluminization pretreatment equipment disclosed in this invention has a stirring shaft on the reactor equipped with spiral blades and spiral strips. The spiral blades can lift the material in the middle upwards, and the spiral strips can push the material at the edge downwards, realizing the up-and-down circulation and comprehensive stirring of the material, avoiding the accumulation of material on the inner wall of the cylinder, so that the antimony concentrate can fully contact the molten salt, significantly improving the uniformity and fullness of the complex desilication and aluminization reaction, effectively improving the desilication and aluminization efficiency, ensuring the purity of the desilication and aluminization antimony concentrate, and providing qualified raw materials for the subsequent preparation of antimony trioxide; 3. The antimony concentrate desilication and aluminization pretreatment equipment disclosed in this invention forms three independent material tanks within the antimony white furnace, separated by weir I and weir II. This allows for segmented temperature control, including preheating at 650℃, oxidation at 720℃, and heat preservation at 780℃. Combined with a fire baffle to cut off the flow of hot air, this ensures stable temperatures in each zone, enabling simultaneous preheating, oxidation, and heat preservation processes. This significantly improves the oxidation and volatilization efficiency of the antimony liquid, increasing the yield and purity of antimony trioxide. The baffle I of the fire baffle can rotate flexibly, effectively blocking hot air flow without obstructing material flow. The structure is simple and highly practical.

[0018] Other advantages, objectives, and features of the invention will be set forth in part in the description which follows, and in part will be apparent to those skilled in the art from the following examination, or may be learned from practice of the invention. The objectives and other advantages of the invention can be realized and obtained through the following description. Attached Figure Description

[0019] To make the objectives, technical solutions, and advantages of the present invention clearer, the preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, wherein: Figure 1 This is a three-dimensional structural schematic diagram of an antimony concentrate desiliconization and aluminization pretreatment device according to the present invention; Figure 2 This is a partial cross-sectional view of the reactor structure of the antimony concentrate desiliconization and aluminization pretreatment equipment of the present invention; Figure 3 This is a partially exploded structural diagram of the cooling mechanism of an antimony concentrate desiliconization and aluminization pretreatment equipment according to the present invention. Figure 4 This is a side view of the cooling cylinder structure of a pretreatment device for desiliconizing and aluminizing antimony concentrate according to the present invention. Figure 5 This is a three-dimensional structural diagram of an antimony white furnace used in the preparation process of antimony trioxide according to the present invention. Figure 6 This is a schematic cross-sectional view of the antimony white furnace used in the antimony trioxide preparation process of the present invention. Figure 7 This is a partial structural diagram of a fire wall according to a process for preparing antimony trioxide according to the present invention; Figure 8 This is a schematic diagram of the material guiding component structure in the antimony trioxide preparation process of the present invention.

[0020] Reference numerals: 1. Reactor; 11. Shell; 12. Jacket; 13. Motor I; 14. Stirring shaft; 15. Feed pipe I; 16. Cover plate; 17. Spiral blade; 18. Spiral strip; 2. Cooling mechanism; 21. Frame; 22. Guide plate I; 23. Guide plate II; 24. Rotating shaft III; 25. Motor II; 26. Inner cylinder; 27. Support ring; 28. Outer cylinder; 29. ​​Rotating ring; 210. Connecting rod; 2 11. Baffle II; 212. Multi-faceted rod; 213. Support rod; 3. Vibrating screen; 4. Antimony white furnace; 41. Burner; 42. Exhaust pipe; 43. Feed pipe II; 44. Hopper; 45. Dike I; 46. Dike II; 47. Feed trough I; 48. Feed trough II; 49. Feed trough III; 5. Firewall; 51. Rotating shaft I; 52. Baffle I; 6. Material guiding assembly; 61. Rotating shaft II; 62. Flip plate; 63. Counterweight. Detailed Implementation

[0021] The following specific examples illustrate the implementation of the present invention. Those skilled in the art can easily understand other advantages and effects of the present invention from the content disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and various details in this specification can be modified or changed based on different viewpoints and applications without departing from the spirit of the present invention. It should be noted that the illustrations provided in the following embodiments are only schematic representations of the basic concept of the present invention. Unless otherwise specified, the following embodiments and features can be combined with each other.

[0022] The accompanying drawings are for illustrative purposes only and are schematic diagrams, not actual pictures. They should not be construed as limiting the invention. To better illustrate the embodiments of the invention, some parts in the drawings may be omitted, enlarged, or reduced, and do not represent the actual product dimensions. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.

[0023] In the accompanying drawings of the embodiments of the present invention, the same or similar reference numerals correspond to the same or similar components. In the description of the present invention, it should be understood that if terms such as "upper," "lower," "left," "right," "front," and "rear" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, they are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the terms used to describe positional relationships in the drawings are only for illustrative purposes and should not be construed as limiting the present invention. For those skilled in the art, the specific meaning of the above terms can be understood according to the specific circumstances.

[0024] Example 1 like Figures 1-4 As shown, an antimony concentrate desilication and aluminization pretreatment device includes a reaction vessel 1 and a vibrating screen 3. The main body of the reaction vessel 1 is a cylinder 11, which is the core reaction chamber of the device, used to contain molten salt, quicklime, and antimony concentrate to complete the complexation and desilication and aluminization reaction. A jacket 12 is fixedly fitted on the outer wall of the cylinder 11, forming a sealed interlayer between the jacket 12 and the outer wall of the cylinder 11, for introducing a heating medium to achieve temperature control of the materials inside the cylinder 11 and ensure that the reaction takes place at a specified temperature. A motor I 13 is fixedly installed at the top of the cylinder 11, providing power for the rotation of a stirring shaft 14. The stirring shaft 14 is rotatably mounted through the top of the cylinder 11 and extends into the interior of the cylinder 11 for stirring the internal materials. A spiral blade 17 is fixed and wound around the bottom end of the stirring shaft 14. The spiral blade 17 rotates with the stirring shaft 14 to lift the materials in the middle of the cylinder 11 upwards, realizing the vertical circulation of the materials and allowing the materials in the middle to be fully mixed with the materials in other areas. A spiral strip 18 is fixedly installed on the outer side of the stirring shaft 14. The outer side of the spiral strip 18 contacts the inner wall of the cylinder 11. During rotation, it pushes the material on the edge of the cylinder 11 downward, preventing the material from accumulating on the inner wall of the cylinder 11. This ensures that all the material in the cylinder 11 is fully stirred, making the reaction more uniform and complete, and improving the desiliconization and aluminum removal effect. The stirring shaft 14, spiral blades 17, and spiral strip 18 are all made of austenitic stainless steel (such as 310S stainless steel) that is resistant to high temperature and molten salt corrosion, or their surfaces are coated with a ceramic protective layer that is resistant to molten salt corrosion. The vibrating screen 3 is a multi-layer linear vibrating screen or circular vibrating screen driven by a vibrating motor. Its interior is fixed with an upper screen with a screen hole size of 2mm and a lower screen with a screen hole size of 0.5mm from top to bottom.

[0025] A feed pipe I15 is fixedly installed through the top of the cylinder 11. The feed pipe I15 is a raw material feeding channel for feeding raw materials such as molten salt, quicklime, and antimony concentrate into the cylinder 11. A cover plate 16 is detachably installed at the top of the feed pipe I15. The cover plate 16 is used to close the feed pipe I15 to prevent material splashing or gas leakage during the reaction process, ensuring the airtightness of the reactor 1. The bottom end of the feed pipe I15 extends into the mixture without affecting the rotation of the spiral strip 18, thus preventing splashing during the feeding process.

[0026] The pretreatment equipment also includes a cooling mechanism 2, which is used to cool and crush the high-temperature mixture discharged from the reactor 1, facilitating the subsequent screening operation of the vibrating screen 3. The bottom of the cooling mechanism 2 is a frame 21, which provides support for all components of the cooling mechanism 2, ensuring stable operation of the entire mechanism. Guide plates I 22 and II 23 are fixed at both ends of the frame 21, respectively. Guide plate I 22 corresponds to the discharge port at the bottom of the reactor 1, and is used to smoothly guide the mixture discharged from the reactor 1 into the cooling cylinder. Guide plate II 23 corresponds to the inlet of the vibrating screen 3, and is used to smoothly guide the cooled and crushed material into the vibrating screen 3, achieving orderly material conveying. The frame 21 contains a rotating cooling cylinder, which is the core component for cooling and crushing. Utilizing its own structural design, the cooling cylinder achieves the dual functions of cooling and crushing materials. The cooling cylinder is equipped with multiple multi-faceted rods 212, which rotate synchronously with the cooling cylinder. As the cooling cylinder rotates, the multi-faceted rods 212, driven by the baffle 211, not only collide with each other and with the inner wall of the inner cylinder 26, but their multi-faceted structure also exerts a continuous squeezing and rubbing effect on the material being cooled during the rolling and sliding process. This achieves efficient crushing of materials that have formed hard shells or lumps, ensuring that the material is crushed to the particle size that meets the screening requirements.

[0027] The cooling cylinder includes two sets of support rods 213, symmetrically distributed, used to fix and support the inner cylinder 26, ensuring that the inner cylinder 26 can rotate synchronously with the rotating shaft Ⅲ 24. The same inner cylinder 26 is fixedly mounted on the outer side of both sets of support rods 213. The inner cylinder 26 serves as a space for material cooling and crushing, where the material undergoes cooling and crushing processes. Support rings 27 are fixedly mounted on the outer walls of both ends of the inner cylinder 26. These support rings 27 connect the inner cylinder 26 and the connecting rods 210, and also provide mounting support for the rotating ring 29. Multiple connecting rods 210 are fixedly mounted between the two support rings 27. An outer cylinder 28 is fixedly fitted onto the outer wall of each connecting rod 210, forming a space for the cooling medium between the outer cylinder 28 and the inner cylinder 26. Cooling of the internal material is achieved by introducing the cooling medium. A rotating ring 29 is rotatably fitted on the outer wall of the support ring 27. The rotating ring 29 and the outer cylinder 28 are connected by a sealing element, which is a dustproof sealing ring, to prevent dust from entering the interior of the cooling cylinder and to reduce the rotational gap. The rotating ring 29 is used to connect the water inlet pipe and the drain pipe to realize the circulation input and discharge of the cooling medium. The two rotating rings 29 are connected to the water inlet pipe and the drain pipe respectively to form a complete cooling medium circulation channel, ensuring that the cooling process continues to be stable.

[0028] A rotating shaft III 24 is rotatably mounted on the top of the frame 21. The rotating shaft III 24 provides support and power transmission for the rotation of the cooling cylinder. Two sets of support rods 213 are fixed to the outer walls of both ends of the rotating shaft III 24, ensuring that the rotating shaft III 24 synchronously drives the cooling cylinder to rotate. A motor II 25 is fixedly mounted on the top side of one side of the frame 21. The motor II 25 provides power for the rotation of the rotating shaft III 24. The motor II 25 is connected to the rotating shaft III 24 via a sprocket and chain, ensuring that the power of the motor II 25 is smoothly transmitted to the rotating shaft III 24, driving the cooling cylinder to rotate at a uniform speed, thus guaranteeing cooling and crushing effects.

[0029] Multiple sets of baffles II211 are fixedly installed on the inner wall of the inner cylinder 26. The baffles II211 rotate synchronously with the cooling cylinder. The rotation of the baffles II211 drives the multi-faceted rod 212 to flip, so that the multi-faceted rod 212 can fully contact the material, improve the crushing efficiency, and at the same time promote the contact between the material and the inner wall of the cooling cylinder, accelerate the cooling speed, and ensure that the material is cooled evenly and crushed thoroughly.

[0030] Example 2 Reference Figures 1-8 A process for preparing antimony trioxide involves processing the raw materials using the aforementioned antimony concentrate desilication and aluminization pretreatment equipment. The specific steps are as follows: S1. The raw material is processed using the aforementioned antimony concentrate desilication and aluminization pretreatment equipment. The core purpose of this step is to remove silicon and aluminum impurities from the antimony concentrate to obtain high-purity desilication and aluminization antimony concentrate, providing qualified raw materials for the subsequent preparation of antimony trioxide. This step specifically includes the following sub-steps, each of which is strictly completed using the corresponding equipment components to ensure that the operation is feasible and the results are guaranteed: S1.1 Molten Salt Preparation: Weigh industrial molten salt according to the ratio of sodium nitrate to potassium chloride = 1:1. After weighing, manually remove the cover plate 16 at the top of the feed pipe I15, and slowly add the weighed industrial molten salt into the cylinder 11 of the reactor 1 through the feed pipe I15. During the addition process, avoid spilling molten salt onto the outer wall of the feed pipe I15 to ensure that all raw materials enter the cylinder 11. After the molten salt is added, add quicklime into the cylinder 11 through the feed pipe I15 at a ratio of 5% of the total mass of the molten salt. The quicklime is used to remove trace impurities in the molten salt and improve the activation effect of the molten salt. After all raw materials have been added, reinstall the cover plate 16 at the top of the feed pipe I15 and tighten it to ensure that the feed pipe I15 is sealed to prevent material splashing or flue gas leakage during subsequent reactions. Subsequently, a heating medium is introduced through the jacket 12 to heat the material inside the cylinder 11. At the same time, the motor I 13 is started, which drives the stirring shaft 14 to rotate. The spiral blades 17 and spiral strips 18 on the stirring shaft 14 rotate synchronously to fully stir the material. After heating to 350°C, this temperature is maintained and stirred continuously for 10 minutes to ensure that the molten salt is completely melted and fully mixed with quicklime to form an activated molten salt system, which is fully prepared for the subsequent complexing and desilication reaction of antimony concentrate.

[0031] S1.2 Antimony Concentrate Complexation and Desilication: After the molten salt system is activated, maintain the circulation of the heating medium in the jacket 12 to keep the temperature inside the cylinder 11 stable at around 350℃, avoiding temperature fluctuations that could affect the reaction. Then, remove the cover plate 16 at the top of the feed pipe I 15 again, and add the antimony concentrate to the cylinder 11 in batches through the feed pipe I 15 at a ratio of molten salt to antimony concentrate of 3:1. The purpose of adding in batches is to avoid adding too much antimony concentrate at once, which could cause material agglomeration, and to ensure that the antimony concentrate can fully contact the activated molten salt to improve the reaction efficiency. The interval between each batch of antimony concentrate is 5 minutes, and the amount added in each batch is controlled within a reasonable range to ensure that after each batch of antimony concentrate is added, it can be quickly and evenly mixed with the molten salt under the stirring action of the stirring shaft 14. After all antimony concentrate has been added, heating continues through jacket 12 to raise the reaction temperature inside cylinder 11 to 380℃. This temperature is the optimal temperature for the complexation and desilication reaction, promoting the full complexation reaction between silicon and aluminum in the antimony concentrate and the molten salt, generating complexes soluble in the molten salt, thereby achieving the separation of silicon and aluminum impurities from antimony. After heating, the temperature is maintained at 380℃ and the stirring shaft 14 is continuously rotated, with continuous stirring for 40 minutes to ensure the reaction proceeds fully and removes silicon and aluminum impurities from the antimony concentrate to the maximum extent. After the reaction, the heating medium is stopped from flowing into jacket 12, and a cooling medium is introduced to cool the material inside cylinder 11. During the cooling process, the stirring shaft 14 is kept rotating to ensure uniform cooling of the material until the material temperature is cooled to below 100℃, preventing high-temperature material from directly entering the cooling mechanism 2, which would overload the cooling mechanism 2 and affect the cooling effect.

[0032] S1.3 Cooling and Crushing of the Mixture: When the material temperature in reactor 1 drops below 100℃, motor I13 is turned off, stirring shaft 14 is stopped, and then the valve at the bottom discharge port of reactor 1 is opened to slowly discharge the mixture prepared in S1.2 (including desilicationized aluminum antimony, silicon-aluminum complex salt, and molten salt). The mixture flows smoothly into the cooling cylinder of cooling mechanism 2 through guide plate I22. The flow rate is controlled during material conveying to avoid excessive material clogging of the cooling cylinder and to ensure that the material enters the cooling cylinder evenly. After all the material has been fed into the cooling cylinder, motor II25 is started. Motor II25 drives shaft III24 to rotate through sprocket and chain. Shaft III24 drives two sets of support rods 213 to rotate synchronously, thereby driving the entire cooling cylinder composed of inner cylinder 26, support ring 27, connecting rod 210 and outer cylinder 28 to rotate. Simultaneously, cooling medium is introduced into the cooling medium's containment space through the water inlet pipe connected to the rotating ring 29. The cooling medium circulates within the containment space between the outer cylinder 28 and the inner cylinder 26, carrying away the heat of the material inside the cooling cylinder through heat conduction, thus achieving material cooling. During the rotation of the cooling cylinder, the baffle II 211 on the inner wall of the inner cylinder 26 rotates synchronously, causing multiple polygonal bars 212 inside the inner cylinder 26 to tumble. During the tumbling process, the polygonal bars 212 repeatedly impact and crush the material during the cooling process, breaking the material clumps formed during the reaction into fine particles, ensuring that the particle size of the material meets the requirements for subsequent screening. The entire cooling and crushing process continues until the material temperature drops to room temperature and the particle size meets the standard for passing through the upper screen of the vibrating screen 3. Then, the motor II 25 and the supply of cooling medium are stopped, and the cooled and crushed material flows smoothly into the feed inlet of the vibrating screen 3 through the guide plate II 23, entering the next screening operation.

[0033] S1.4 Vibrating Screen Grading: Start vibrating screen 3. Vibrating screen 3 begins to vibrate. Slowly pour the cooled and crushed material into the feed inlet of vibrating screen 3. Under the vibration of vibrating screen 3, the material flows downward along the screen mesh for grading and screening. Vibrating screen 3 is set with two layers. The upper screen is used to intercept coarse particles with a particle size greater than 2mm. These coarse particles are mainly unreacted antimony concentrate lumps and cannot enter the subsequent preparation steps. They need to be discharged through the coarse material outlet of vibrating screen 3. After discharge, they are conveyed to feed pipe I15 by a conveying device and added back to reactor 1 for secondary treatment to ensure full utilization of raw materials and avoid waste. The middle layer material is silicon-aluminum complex salt with a particle size between 0.5-2mm. This part of the material is an impurity product generated during the desiliconization process. It can be discharged through the middle material outlet of vibrating screen 3 and collected for sale as building auxiliary materials, realizing resource recycling. The lower layer material consists of desilicationized aluminum-antimony concentrate with a particle size of less than 0.5 mm. This material is a qualified pre-treated raw material, which is discharged through the fine material outlet of vibrating screen 3 and collected for later use in the preparation of antimony trioxide. After screening, vibrating screen 3 is turned off, and the residual material on the screen is cleaned to avoid affecting the screening effect of the next screening and to ensure that each batch of screening can be accurately graded.

[0034] S2. Oxidation Preparation of Antimony Trioxide: After step S1, qualified desilicationized aluminum antimony concentrate is obtained, and the core preparation step of antimony trioxide begins. This step is completed using the antimony white furnace 4, and the specific operation is as follows: Start the antimony white furnace 4, prepare for preheating inside the furnace, and ensure that the antimony white furnace 4 can operate stably. A burner 41 is fixedly installed through one side of the antimony white furnace 4. After the burner 41 is started, it provides the high-temperature heat required for the reaction in the antimony white furnace 4. The burner 41 extends into the material tank Ⅲ 49 to ensure that the heat can directly act on the material and improve heating efficiency. To adapt to the high-temperature working environment, the part of the burner 41 extending into the antimony white furnace 4 is fitted with a heat insulation sleeve to avoid the high temperature directly acting on the burner 41. An exhaust pipe 42 is fixedly installed through the top of the antimony white furnace 4. The exhaust pipe 42 is used to discharge the flue gas generated in the furnace reaction, ensuring that the flue gas can be discharged in a timely manner to avoid excessive pressure in the furnace, and at the same time providing a channel for subsequent flue gas treatment and antimony white collection. The top of the antimony white furnace 4 is fixedly equipped with a feed pipe II 43. The top of the feed pipe II 43 is connected to two hoppers 44. The two hoppers 44 are used to load desilication aluminum antimony concentrate and refined antimony blocks respectively. The feed is carried out at a ratio of desilication aluminum antimony concentrate to refined antimony blocks = 1:3. This ratio can ensure that the antimony liquid oxidation reaction is sufficient and improve the yield and purity of antimony trioxide.

[0035] The bottom wall of the antimony white furnace 4 is fixedly equipped with cofferdam I 45 and cofferdam II 46. Cofferdam I 45 and cofferdam II 46 divide the furnace chamber of the antimony white furnace 4 into three independent material troughs. Material trough I 47 is formed inside cofferdam II 46, material trough II 48 is formed between cofferdam II 46 and cofferdam I 45, and material trough III 49 is formed between cofferdam I 45 and the antimony white furnace 4. The three material troughs are arranged in a ring and the height decreases in a stepped manner from the inside to the outside, which facilitates the sequential flow of materials and realizes segmented temperature control. Burner 41 extends into material tank III 49 to heat the material inside, maintaining the temperature of material tank III 49 at 780℃ for material insulation and ensuring that the antimony liquid remains in a molten state; the temperature of material tank II 48 is maintained at 720℃ for the oxidation reaction of antimony liquid, allowing the antimony liquid to fully react with preheated air to generate antimony trioxide; the temperature of material tank I 47 is maintained at 650℃ for preheating the material, allowing the material to gradually adapt to the high-temperature environment and avoiding sudden temperature rise that could cause the material to clump together and affect the reaction effect.

[0036] A fire baffle 5 is installed inside the antimony white furnace 4. The fire baffle 5 is used to cut off the airflow below between material troughs I 47 and II 48, and between material troughs II 48 and III 49, to prevent the hot airflow from moving between different temperature zones, ensuring the temperature stability of each material trough and providing a stable temperature environment for the reaction. The fire baffle 5 includes two sets of rotating shafts I 51 fixed to the top of the antimony white furnace 4. The two sets of rotating shafts I 51 correspond to the boundaries between material troughs I 47 and II 48, and between material troughs II 48 and III 49, respectively. The bottom end of the rotating shafts I 51 is fitted with baffles I 52. The height of the two sets of baffles I 52 is adapted to the cofferdams I 45 and II 46, respectively, to ensure that the baffles I 52 can effectively block the hot airflow, while not hindering the orderly flow of materials between the three material troughs.

[0037] During the feeding process, the guiding component 6 inside the feed pipe II 43 plays a role. The guiding component 6 includes a rotating shaft II 61, which is fixedly installed on the inner wall of the feed pipe II 43. The outer wall of the rotating shaft II 61 is fitted with an inclined flap 62. When the material on one side of the flap 62 accumulates to a certain weight, the weight of the material is greater than the resistance of the flap 62, naturally pushing the flap 62 open, and the material falls smoothly into the corresponding material trough inside the antimony white furnace 4. A counterweight 63 is fixedly installed at the bottom of one side of the flap 62. When the flap 62 flips and the material falls, the flap 62 automatically resets and flips under the gravity of the counterweight 63, closing the feed channel, preventing hot gas backflow or material splashing in the furnace, and ensuring a stable and orderly feeding process.

[0038] After the feed is stabilized, preheated air is blown into the antimony white furnace 4. The preheated air comes into full contact with the molten antimony in the furnace 4, causing the antimony liquid to undergo an oxidation and volatilization reaction, generating antimony trioxide flue gas. The generated antimony trioxide flue gas is discharged from the antimony white furnace 4 through exhaust pipe 42 and enters the subsequent rapid cooling device, cyclone classifier, and bag dust collector. Rapid cooling quickly lowers the flue gas temperature to prevent excessive crystallization of antimony trioxide. Cyclone classification removes coarse particulate impurities from the flue gas. The bag dust collector intercepts and collects the antimony trioxide powder, yielding crude antimony trioxide product.

[0039] S3. Product Testing: Strict testing is conducted on the antimony trioxide powder collected by the baghouse dust collector to ensure product quality meets industry standards. The specific testing process is as follows: First, an appropriate amount of antimony trioxide powder sample is taken, and the specific gravity of the product is measured using a hydrometer. The acceptable standard is a specific gravity ≥ 5.1 g / cm³. 3 If the measurement results are not up to standard, it indicates that there are impurities in the product. The unqualified product needs to be returned to the antimony white furnace 4 for re-oxidation reaction. Secondly, the particle size of the product is measured using a 2μm standard sieve. An appropriate amount of sample is placed in the standard sieve for sieving test. The qualified standard is that the material passing through the sieve is ≥98%. If the particle size is not up to standard, the cooling speed of the rapid cooling device needs to be adjusted and the product needs to be re-prepared. Only antimony trioxide powder that meets the qualified standards in terms of specific gravity and particle size can be packaged and stored as a qualified product. Unqualified products need to be reprocessed to ensure that the quality of the products leaving the factory meets the standards.

[0040] S4. Molten Salt Recycling: To reduce production costs and improve resource utilization, the molten salt after reaction in the antimony white furnace 4 is recycled. The specific operation is as follows: After the oxidation reaction in the antimony white furnace 4 is completed, the burner 41 and the preheated air supply are turned off. After the temperature inside the antimony white furnace 4 drops to a safe range, the discharge port at the bottom of the antimony white furnace 4 is opened to collect the molten salt after reaction. The collected molten salt is poured into a cooling container and allowed to cool naturally to room temperature. During the cooling process, the molten salt is constantly turned to prevent it from clumping. After cooling to room temperature, the molten salt is sieved through a standard sieve to remove impurities (mainly unreacted residue). The sieved molten salt is then placed in a stirring device, and 5% new molten salt is added. The ratio of the new molten salt is consistent with that in S1.1, i.e., sodium nitrate: potassium chloride = 1:1. The stirring device is started to thoroughly mix the new molten salt with the recycled molten salt. After thorough mixing, the molten salt is added to the reactor 1 through the feed pipe I15 for reuse in the pretreatment of antimony concentrate.

[0041] It should be noted that a guiding component 6 is also provided inside the feed pipe I 15, and its structure is completely identical to that of the guiding component 6 inside the feed pipe II 43, both including a rotating shaft II 61, a flap 62, and a counterweight 63. The rotating shaft II 61 is fixedly installed on the inner wall of the feed pipe I 15, the flap 62 is tilted and rotated on the outer wall of the rotating shaft II 61, and the counterweight 63 is fixed to the bottom of one side of the flap 62. When raw materials are added to the reactor 1 through the feed pipe I 15, the material accumulates on one side of the flap 62. After reaching a certain gravity, the flap 62 is pushed open, and the material falls smoothly into the cylinder 11. After the material falls, the flap 62 automatically resets under the gravity of the counterweight 63, closing the feed channel and preventing the backflow of flue gas or material in the reactor 1, ensuring a stable feeding process. At the same time, no additional power is required, making the structure simple and highly practical.

[0042] This equipment is also equipped with a PLC controller (the model is only an example and is not limited to this). The PLC controller is electrically connected to motor I13, motor II25, burner 41 and various valves. It can preset programs to control the start and stop of motor I13 and its speed to adjust the stirring effect, control the speed of motor II25 to adjust the rotation speed of the cooling cylinder, control the heating power of burner 41 to achieve segmented temperature control of the antimony white furnace, and control the opening and closing sequence of various discharge and feed valves to ensure that the pretreatment and preparation processes are carried out in an orderly manner. In addition, all exposed transmission components (rotating shaft III, the passage of the stirring shaft, and the rotating ring) are equipped with dustproof structures. The passage between the stirring shaft and the cylinder is equipped with a dustproof sealing sleeve, the connection between rotating shaft III and the frame is equipped with a dustproof cover, and the connection between the rotating ring and the outer cylinder is equipped with a dustproof sealing ring. This can effectively prevent dust from entering the gaps between components, avoid equipment jamming and wear, and extend the service life of the equipment.

[0043] However, as is well known to those skilled in the art, the working principles and wiring methods of motor I13, motor II25 and burner 41 are all conventional methods or common knowledge, and will not be described in detail here. Those skilled in the art can make any selections according to their needs or convenience.

[0044] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A pretreatment device for desilication and aluminization of antimony concentrate, comprising a reactor (1) and a vibrating screen (3), wherein the reactor (1) comprises a cylinder (11), a jacket (12) is fixedly fitted on the outer wall of the cylinder (11), a motor I (13) is fixedly fitted on the top of the cylinder (11), a stirring shaft (14) is rotatably fitted through the top of the cylinder (11), a feed pipe I (15) is fixedly fitted through the top of the cylinder (11), and a cover plate (16) is detachably fitted on the top of the feed pipe I (15). Its features are, It also includes a cooling mechanism (2), which includes a frame (21). The two ends of the frame (21) are respectively fixed with guide plate I (22) and guide plate II (23). The guide plate I (22) corresponds to the discharge port at the bottom of the reactor (1), and the guide plate II (23) corresponds to the feed port of the vibrating screen (3). A cooling cylinder rotates inside the frame (21) to cool the material. The cooling cylinder is provided with multiple multi-faceted bars (212). When the cooling cylinder rotates, the multi-faceted bars (212) are used to crush the cooled material.

2. The antimony concentrate desilication and aluminization pretreatment equipment according to claim 1, characterized in that, The bottom end of the stirring shaft (14) is fixed and has a spiral blade (17) wrapped around it. The spiral blade (17) is used to lift the material in the middle upward. A spiral strip (18) is fixed on the outside of the stirring shaft (14). The outside of the spiral strip (18) contacts the inner wall of the cylinder (11). During the rotation, the material on the edge is pushed downward.

3. The antimony concentrate desilication and aluminization pretreatment equipment according to claim 1, characterized in that, The cooling cylinder includes two sets of support rods (213). The same inner cylinder (26) is fixedly provided on the outer side of the two sets of support rods (213). Support rings (27) are fixedly provided on the outer walls of both ends of the inner cylinder (26). Multiple connecting rods (210) are fixedly provided between the two support rings (27). The multiple connecting rods (210) are used to support the outer cylinder (28). The outer cylinder (28) is fixedly sleeved on the outer wall of the multiple connecting rods (210), and a space for accommodating the cooling medium is formed between the outer cylinder (28) and the inner cylinder (26). A rotating ring (29) is rotatably sleeved on the outer wall of the support ring (27). The rotating ring (29) is rotatably connected to the outer cylinder (28). The two rotating rings (29) are respectively connected to the water inlet pipe and the water outlet pipe.

4. The antimony concentrate desilication and aluminization pretreatment equipment according to claim 3, characterized in that, The top of the frame (21) is rotatably provided with a rotating shaft III (24), and two sets of support rods (213) are respectively fixed to the outer walls of the two ends of the rotating shaft III (24). A motor II (25) is fixedly provided on the top of one side of the frame (21), and the motor II (25) is connected to the rotating shaft III (24) through a sprocket and a chain.

5. The antimony concentrate desilication and aluminization pretreatment equipment according to claim 3, characterized in that, The inner wall of the inner cylinder (26) is fixedly provided with multiple sets of baffles II (211), which drive the multi-faceted rod (212) to flip.

6. A process for preparing antimony trioxide, characterized in that, Includes the following steps: S1. Processing the raw material using the antimony concentrate desilication and aluminization pretreatment equipment as described in any one of claims 1-5: S1.1, Molten salt preparation: Weigh industrial molten salt according to the ratio of sodium nitrate: potassium chloride = 1:1, add it into the reaction vessel (1), add 5% quicklime, heat to 350℃ to melt and stir to activate for 10 minutes; S1.2, Antimony concentrate complexation and desilication: According to the ratio of molten salt: antimony concentrate = 3:1, antimony concentrate is added to the reactor (1) in batches, heated to 380℃ and stirred for 40 minutes, and then cooled to below 100℃; S1.3, Cooling and Crushing of the Mixture: The mixture prepared in S1.2 is placed in the cooling mechanism (2) for cooling and crushing; S1.4, Vibrating screen grading: The cooled material is poured into the vibrating screen (3), which includes two layers of vibrating screen (upper layer 2mm, lower layer 0.5mm). The desiliconized aluminum antimony concentrate below 0.5mm in the lower layer is collected, and the coarse particles in the upper layer are returned to the reactor (1) for secondary treatment. S2. Start the antimony white furnace (4), feed the desilication aluminum antimony concentrate: refined antimony blocks = 1:3, control the temperature in stages (650℃ preheating, 720℃ oxidation, 780℃ heat preservation), blow in preheated air to oxidize and volatilize the antimony liquid, and the flue gas is rapidly cooled, cyclone graded, and bagged to obtain antimony trioxide powder. S3. Product testing: measure the specific gravity of the product with a hydrometer (≥5.1g / cm 3 is qualified), measure the particle size with a 2μm standard sieve (≥98% of undersize is qualified); S4. Molten salt recycling: Molten salt is recovered from the antimony white furnace (4), cooled and sieved, and 5% new molten salt is added and reused for the pretreatment of antimony concentrate.

7. The process for preparing antimony trioxide according to claim 6, characterized in that, The antimony white furnace (4) includes a burner (41) that is fixed through one side of the antimony white furnace (4), an exhaust pipe (42) that is fixed through the top of the antimony white furnace (4), a feed pipe II (43) that is fixed through the top of the antimony white furnace (4), and two hoppers (44) connected to the top of the feed pipe II (43). It also includes a cofferdam I (45) and a cofferdam II (46) fixed to the bottom wall of the antimony white furnace (4), wherein a material trough I (47) is formed inside the cofferdam II (46), a material trough II (48) is formed between the cofferdam II (46) and the cofferdam I (45), and a material trough III (49) is formed between the cofferdam I (45) and the antimony white furnace (4), wherein the burner (41) extends into the material trough III (49); It also includes a firebreak wall (5), which is installed inside the antimony white furnace (4) to cut off the airflow between material trough I (47) and material trough II (48) and between material trough II (48) and material trough III (49) to prevent hot airflow from spreading.

8. The process for preparing antimony trioxide according to claim 7, characterized in that, The fire wall (5) includes two sets of rotating shafts I (51) fixed to the top of the antimony white furnace (4). The bottom end of the rotating shaft I (51) is fitted with a baffle I (52). The heights of the two sets of baffles I (52) are adapted to the cofferdam I (45) and cofferdam II (46) respectively.

9. The process for preparing antimony trioxide according to claim 6, characterized in that, Both feed pipe I (15) and feed pipe II (43) are provided with a guide assembly (6). The guide assembly (6) includes a rotating shaft II (61). The outer wall of the rotating shaft II (61) is rotatably fitted with an inclined flap (62).

10. The process for preparing antimony trioxide according to claim 9, characterized in that, A counterweight (63) is fixedly provided on one side of the bottom of the flip plate (62). When the flip plate (62) flips and the material falls, it can be reset and flipped under the gravity of the counterweight (63).

Images