Method for preparing sodium fluosilicate from copper smelting arsenic removal waste acid and aging container

By converting fluoride in copper smelting waste acid into fluorosilicate and reacting with sodium sulfate to prepare sodium fluorosilicate, the problem of stagnation of the preparation method of sodium fluorosilicate in the prior art is solved, and efficient removal and recycling are achieved The fluorine in waste acid improves resource utilization and product purity.

CN119390073APending Publication Date: 2025-02-07CHIFENG JINJIAN COPPER IND CO LTD
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Patent Information

Application Number
CN202411529339.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-30
Publication Date
2025-02-07

AI Technical Summary

Technical Problem

The existing preparation methods for sodium fluorosilicate have stagnated production technology, and there are few researches on the treatment, recycling and reuse of waste acid in copper smelting, resulting in low resource utilization efficiency and serious environmental pollution.

Method used

After filtering the fluorine-containing waste acid of copper smelted after desorption, silica is added for heating and stirring reaction to produce fluorosilicate, and then a saturated liquid of sodium sulfate is added to prepare sodium fluorosilicate and aging is performed by aging. High purity sodium fluorosilicate is obtained.

Benefits of technology

It realizes efficient removal and recycling of fluorine in waste acid, reduces environmental pollution, improves resource utilization, and obtains high-purity sodium fluorosilicate.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a method for preparing sodium fluosilicate by using copper smelting arsenic-removed waste acid and an aging container, and the method comprises the following steps: S1, filtering the arsenic-removed fluorine-containing waste acid, and then placing the arsenic-removed fluorine-containing waste acid in a reaction tank I to remove solid particles and impurities in the waste acid; s2, adding silicon dioxide, heating, stirring and reacting for 0.5-1 hour, converting fluoride in the waste acid to produce fluosilicic acid, and filtering a reaction product; s3, conveying the generated fluosilicic acid into a reaction tank II, adding a proper amount of sodium sulfate saturated liquid, and preparing sodium fluosilicate; s4, carrying out aging treatment; and S5, washing and drying the generated sodium fluosilicate precipitate to obtain a final product. According to the method, high-purity sodium fluosilicate is prepared from the fluorine-containing waste acid in copper smelting, and fluorine in the waste acid is efficiently removed and recycled, so that pollution to the environment is reduced, and the resource utilization rate is increased.
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Description

Technical Field

[0001] The invention relates to the technical field of sodium fluorosilicate preparation, and in particular to a method for preparing sodium fluorosilicate by utilizing waste acid from copper smelting and arsenic removal, and an aging container. Background Art

[0002] Sodium fluorosilicate can be used as enamel opalizer, cosolvent, agricultural pesticide and defoliant, hygroscopic agent for acid-resistant cement, animal glue, leather and wood preservative, drinking water treatment agent, manufacturing of opal glass, acid-resistant concrete and acid-resistant cement coagulant in the construction industry, filler for plastics, and used in medicine, rubber, artificial marble, etc. However, domestic sodium fluorosilicate manufacturers generally have stagnant production technology. At present, there are two main methods for preparing sodium fluorosilicate in China. At present, there are two main methods for preparing sodium fluorosilicate in China. One is the neutralization method, that is, sodium carbonate or sodium hydroxide is used to directly neutralize fluorosilicic acid; the other is the phosphate fertilizer by-product method, that is, the fluorine-containing waste gas generated in the production process of wet phosphoric acid is absorbed with water, and then reacted with sodium chloride.

[0003] Waste acid produced during copper smelting contains a large amount of arsenic and fluoride. The sodium hydrosulfide treatment process can make the waste acid meet the reuse standards, but there are still harmful substances such as arsenic and fluorine. During the copper smelting acid production process of our company, a large amount of arsenic-containing waste acid is produced, with an arsenic content of 5000-15000 mg / L and a fluorine content of 1000-2000 mg / L. Based on the annual output of 500,000 tons of cathode copper in copper smelting, about 2000-2500 tons of waste acid are produced every day. By preparing sodium fluorosilicate, the fluorine valuable metal in the waste acid can be recovered, and the amount of limestone used can be effectively reduced, thereby improving resource utilization efficiency.

[0004] The composition of waste acid is shown in the following table:

[0005]

[0006] There are two main methods for preparing sodium fluorosilicate in China: neutralization method and phosphate fertilizer by-product method. Both methods are carried out in aqueous solution and produce a large amount of industrial wastewater.

[0007] With the continuous development and progress of the copper smelting industry, various research results have revolutionized copper smelting technology in China and the world. However, most of the research on copper smelting technology improvement is aimed at purifying copper, but there are few studies on the treatment and recycling of waste acid in the copper smelting industry. At present, the treatment method of copper smelting enterprises for waste acid generated in the production process is basically to use sodium hydrosulfide dearsenicization, calcium carbonate deacidification, and calcium hydroxide defluorination process. The reaction equation is shown in the table below.

[0008] Sodium Hydrosulfide Arsenic Removal

[0009] 2NaHS+H2SO4=Na2SO4+2H2S

[0010] 2HAsO2+3H2S=As2S3↓+4H2O

[0011] 2H3AsO4+5H2S=As2S3↓+2S+8H20

[0012] Calcium carbonate deacidification

[0013] CaCO3+H2SO4→CaSO4+CO2+H2O

[0014] Calcium hydroxide defluorination

[0015] Ca(OH)2+2HF→CaF2+2H2O

[0016] In view of the above content, the research on preparing sodium fluorosilicate using copper smelting waste acid is not yet mature and there is a lot of room for research. Therefore, the present application provides a method for preparing sodium fluorosilicate using copper smelting dearsenication waste acid and an aging container to meet the needs. Summary of the invention

[0017] The purpose of the present application is to provide a method and an aging container for preparing sodium fluorosilicate using waste acid from copper smelting for arsenic removal, and to prepare high-purity sodium fluorosilicate using waste acid containing fluorine from copper smelting, thereby achieving efficient removal and recovery of fluorine in the waste acid, thereby reducing pollution to the environment and improving resource utilization.

[0018] To achieve the above-mentioned purpose, the present application provides the following technical solution: a method for preparing sodium fluorosilicate using waste acid from copper smelting and arsenic removal and an aging container, characterized in that it comprises the following steps:

[0019] S1: filtering the fluorine-containing waste acid after arsenic removal and placing it in a reaction tank 1, wherein the filtration is to remove solid particles and impurities in the waste acid;

[0020] S2: Add silicon dioxide, heat and stir to react for 0.5 to 1 hour, convert the fluoride in the waste acid to produce fluorosilicic acid, and filter the reaction product;

[0021] S3: transporting the generated fluorosilicic acid to the second reaction tank, adding an appropriate amount of saturated sodium sulfate liquid to prepare sodium fluorosilicate;

[0022] S4: aging treatment, the product in the reaction tank 2 in step S3 is transported to an aging container for aging treatment, and filtered after aging. The temperature during aging is controlled at 25°C-65°C. The temperature control is divided into three stages. The aging time is 4 to 6 hours, and stirring is performed every 0.5 hours. The temperature control includes the following stages;

[0023] S41: In the first temperature control stage, the temperature is controlled at 25°C-30°C for 1 to 2 hours;

[0024] S42: The second temperature control stage, the temperature is controlled at 45°C-50°C, and the duration is 1 to 2 hours;

[0025] S43: The third temperature control stage, the temperature is controlled at 60℃-65℃; the duration is 1 to 2 hours;

[0026] S5: washing and drying the produced sodium fluorosilicate precipitate to obtain a final product.

[0027] An aging container, applied to a method for preparing sodium fluorosilicate by using waste acid from copper smelting for arsenic removal as described in the claim, comprising an O-shaped electric track with multiple electric sliders, each of the multiple electric sliders is provided with a driving cylinder, and each of the output ends of the driving cylinder is provided with a storage barrel, and three groups of thermostatic barrels are sequentially arranged side by side below the storage barrel, namely a first thermostatic barrel, a second thermostatic barrel and a third thermostatic barrel;

[0028] The inner cavity of the storage barrel is provided with a stirring shaft driven by a motor, and the lower end of the discharge barrel is provided with a liquid outlet pipe with an electric valve;

[0029] The upper ends of the first constant temperature barrel, the second constant temperature barrel and the third constant temperature barrel are all open, the first constant temperature barrel is connected to the chiller through a connecting pipe, the inner walls of the second constant temperature barrel and the third constant temperature barrel are provided with electric heating pipes, and the motor, the electric valve, the chiller, the electric heating pipe, the drive cylinder and the O-shaped electric track are all electrically connected to the PLC controller

[0030] As a preferred implementation manner in this embodiment, it also includes a first sealing unit, which seals the openings of the three groups of constant temperature barrels, and automatically releases the cover on the openings or automatically covers the openings when the storage barrel enters or moves out of the first constant temperature barrel, the second constant temperature barrel and the third constant temperature barrel.

[0031] As a preferred implementation in this embodiment, the first sealing unit includes two movable feed plates respectively mounted on the corresponding semi-annular plates of the first constant temperature barrel, the second constant temperature barrel and the third constant temperature barrel, and fixed plates mounted on the two side walls of the first constant temperature barrel, the second constant temperature barrel and the third constant temperature barrel, the movable feed plate is composed of two symmetrically connected semi-conical hollow circular tubes, the upper ends of the two semi-annular plates are fixed with sleeves, and the sleeves are slidably sleeved on the corresponding limiting rods, and the two ends of the limiting rods are respectively fixedly connected to the two fixed plates;

[0032] A slide plate slidably connected to the corresponding fixed plate is fixed on each of the two semi-annular plates, and a first mounting block with an inclined surface is provided on both side ends of the slide plate, and a plurality of second mounting blocks with inclined surfaces are provided in a straight line on the fixed plate and on both sides of the slide plate, the inclined surface of the first mounting block is opposite to and parallel to the inclined surface of the second mounting block, a first permanent magnet is provided on the inclined surface of the first mounting block, and a second permanent magnet is provided on the inclined surface of the second mounting block, and the first permanent magnet and the second permanent magnet have the same magnetic poles at opposite ends;

[0033] An upper conical guide portion and a lower conical guide portion are respectively arranged at the upper and lower ends of the material storage barrel, and a plurality of material feeding openings are arranged on the upper conical guide portion.

[0034] As a preferred implementation mode in this embodiment, it also includes a second sealing unit, which automatically seals or releases the seal of the cavity formed between the two movable feed plates without affecting the movement of the storage barrel in and out of the first constant temperature barrel, the second constant temperature barrel and the third constant temperature barrel.

[0035] As a preferred implementation in this embodiment, the second sealing unit includes an upper blocking plate and a lower bottom plate with water flow holes connected together by a connecting rod, and T-shaped rods slidably connected to the corresponding inner walls of the constant temperature barrel are fixed on both side walls of the lower bottom plate;

[0036] Two guide wheel assembly mounting frames are symmetrically arranged on the outer wall of the thermostatic barrel, and both guide wheel assemblies are equipped with pull ropes, and one end of the two pull ropes is respectively connected to the corresponding T-shaped rods, and the other end of the two pull ropes is connected to the weights.

[0037] As a preferred implementation manner in this embodiment, the diameter of the smallest circular cavity formed between the two movable feed plates is consistent with the diameter of the output end of the driving cylinder.

[0038] In summary, the technical effects and advantages of the present invention are as follows:

[0039] 1. This method utilizes fluorine-containing waste acid from copper smelting to prepare high-purity sodium fluorosilicate, achieving efficient removal and recovery of fluorine in the waste acid, thereby reducing environmental pollution and improving resource utilization.

[0040] 2. In the present invention, a first sealing unit and a second sealing unit are arranged on the aging container, and the constant temperature barrel is automatically sealed after the storage barrel enters or moves out of the constant temperature barrel. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without paying any creative work.

[0042] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0043] Figure 2 for Figure 1 The middle constant temperature barrel and the partial enlarged structure diagram;

[0044] Figure 3 for Figure 2 Schematic diagram of the second permanent magnet installation structure;

[0045] Figure 4 for Figure 2 Schematic diagram of the partial split structure of the medium constant temperature barrel;

[0046] Figure 5 for Figure 4 A schematic diagram of the structure of the second sealing unit;

[0047] Figure 6 for Figure 1 Schematic diagram of the structure of the medium storage barrel.

[0048] In the figure: 1. O-shaped electric track; 2. electric slider; 3. driving cylinder; 4. storage barrel; 41. lower conical guide; 42. upper conical guide; 43. feeding opening; 44. stirring shaft; 45. liquid outlet pipe; 5. first constant temperature barrel; 6. second constant temperature barrel; 7. third constant temperature barrel; 8. semi-ring plate; 9. movable feed plate; 10. slide plate; 11. first permanent magnet; 12. second permanent magnet; 13. limit rod; 14. sleeve; 15. upper blocking plate; 16. connecting rod; 17. lower bottom plate; 18. T-shaped rod; 19. guide wheel group; 20. mounting frame; 21. pull rope; 22. weight; 23. fixing plate. DETAILED DESCRIPTION

[0049] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0050] A method for preparing sodium fluorosilicate using waste acid from copper smelting and arsenic removal and an aging container, comprising the following steps:

[0051] S1: filtering the fluorine-containing waste acid after arsenic removal and placing it in a reaction tank 1, wherein the filtration is to remove solid particles and impurities in the waste acid;

[0052] S2: Add silicon dioxide, heat and stir to react for 0.5 to 1 hour, convert the fluoride in the waste acid to produce fluorosilicic acid, and filter the reaction product;

[0053] S3: transporting the generated fluorosilicic acid to the second reaction tank, adding an appropriate amount of saturated sodium sulfate liquid to prepare sodium fluorosilicate;

[0054] S4: aging treatment, the product in the reaction tank 2 in step S3 is transported to an aging container for aging treatment, and filtered after aging. The temperature during aging is controlled at 25°C-65°C. The temperature control is divided into three stages. The aging time is 4 to 6 hours. Stirring is performed every 0.5 hours. The stirring can prevent agglomeration and also help heat transfer. The temperature control includes the following stages;

[0055] S41: In the first temperature control stage, the temperature is controlled at 25°C-30°C for 1 to 2 hours;

[0056] S42: The second temperature control stage, the temperature is controlled at 45°C-50°C, and the duration is 1 to 2 hours;

[0057] S43: The third temperature control stage, the temperature is controlled at 60℃-65℃; the duration is 1 to 2 hours;

[0058] S5: washing and drying the produced sodium fluorosilicate precipitate to obtain a final product.

[0059] The method adopts the method of adding sodium sulfate and quartz sand to efficiently remove fluoride in the waste acid, and utilizes sodium sulfate saturated liquid to react with fluosilicic acid to prepare sodium fluosilicate and recover fluorine in the waste acid. The sodium sulfate saturated liquid can provide sufficient sodium ions in the reaction process, and after combining with fluosilicic acid, sodium fluosilicate precipitation is formed. Since the solution is already in a saturated state, it is easier to promote the precipitation and growth of crystals. At the same time, the use of sodium sulfate saturated liquid can reduce the generation of impurities in the reaction process. This is because the solubility of the solute in the saturated solution has reached a limit, so it is difficult to dissolve other impurity ions, thereby ensuring the purity of the product (that is, high-purity sodium fluosilicate can be obtained by adopting this process);

[0060] The aging process is divided into three stages of temperature control. The temperature of the first stage is controlled at 25℃-30℃. Within this temperature range, a lower temperature helps to reduce the solubility of the solute in the solution, thereby reducing the impurity content and creating a purer environment for the subsequent crystal precipitation; the lower temperature slows down the rate of chemical reactions, allowing the ions in the solution to have enough time to arrange in order, forming a relatively complete crystal structure, and improving the quality and purity of the Na2SiF6 crystals;

[0061] The temperature in the second stage is controlled at 45℃-50℃. As the temperature rises, the reaction rate accelerates, which is conducive to the rapid growth and precipitation of crystals. Within this temperature range, crystals can grow in an orderly manner according to their inherent crystal structure to form a regular and complete crystal morphology, which helps to improve the purity and crystallinity of the product. This stage of temperature control helps to balance the effects of reaction rate and impurities. Although the increase in temperature may increase the solubility of some impurities, it also promotes the growth of crystals, thereby offsetting the negative effects of impurities to a certain extent.

[0062] The temperature of the third stage is controlled at 60℃-65℃ (it should be noted that too high a temperature may cause the crystal to grow too fast, resulting in irregular crystal morphology and increased defects, which will affect the purity and quality of the product, and maintaining a higher aging temperature requires more energy consumption, which will increase production costs). At this temperature stage, the defects and stresses inside the crystal are further released and adjusted, making the crystal more perfect and stable. This process is called crystal maturation. The matured crystal has higher purity and better physical properties. Higher temperatures help reduce the adsorption of impurity ions in the solution on the crystal surface, thereby reducing the impurity content in the product. At the same time, high temperatures can also promote the dissolution and discharge of impurities, further improving the purity of the product.

[0063] The method utilizes fluorine-containing waste acid from copper smelting to prepare high-purity sodium fluorosilicate, thereby achieving efficient removal and recovery of fluorine in the waste acid, thereby reducing pollution to the environment and improving resource utilization.

[0064] like Figure 1 As shown, an aging container is applied to a method for preparing sodium fluorosilicate using waste acid from copper smelting for arsenic removal according to claim 1, comprising an O-shaped electric track 1 with multiple electric sliders 2, each of which is provided with a driving cylinder 3, and each of which is provided with a storage barrel 4 at the output end of the driving cylinder 3, and three groups of constant temperature barrels are sequentially arranged side by side below the storage barrel 4, namely a first constant temperature barrel 5, a second constant temperature barrel 6 and a third constant temperature barrel 7;

[0065] The inner cavity of the storage barrel 4 is provided with a stirring shaft 44 driven by a motor, and the lower end of the discharge barrel 4 is provided with a liquid outlet pipe 45 with an electric valve;

[0066] The upper ends of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7 are all open. The first constant temperature barrel 5 is connected to the chiller through a connecting pipe. Electric heating pipes are provided on the inner walls of the second constant temperature barrel 6 and the third constant temperature barrel 7. The motor, electric valve, chiller, electric heating pipe, drive cylinder and O-shaped electric track 1 are all electrically connected to the PLC controller.

[0067] Three constant temperature barrels are set up, and the storage barrel 4 filled with materials is placed in three groups of constant temperature barrels in turn through the driving cylinder 3 for aging treatment in different temperature control stages. The first constant temperature barrel 5 corresponds to the first temperature control stage, the second constant temperature barrel 6 corresponds to the second temperature control stage, and the third constant temperature barrel 7 corresponds to the third temperature control stage. A chiller is used to inject condensed water into the first constant temperature barrel 5 and maintain the internal constant temperature. The water in the second constant temperature barrel 6 and the third constant temperature barrel 7 is heated by an electric heating pipe so that it reaches the set temperature and is subjected to constant temperature treatment. After the aging treatment is completed, the storage barrel 4 can be moved out of the constant temperature barrel by the driving cylinder 3 and discharged to a designated location through an electric valve.

[0068] It should be noted that the barrel bodies of the three groups of constant temperature barrels are all made of heat-insulating materials, and the barrel body of the storage barrel 4 is made of heat-conducting metal material.

[0069] As a preferred implementation manner in this embodiment, it also includes a first sealing unit, which seals the openings of the three groups of constant temperature barrels, and automatically releases the cover on the openings or automatically covers the openings when the storage barrel 4 enters or moves out of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7.

[0070] As a preferred implementation in this embodiment, Figure 1-3 and Figure 6 As shown, the first sealing unit includes two movable feed plates 9 respectively mounted on the semi-ring plates 8 of the corresponding first thermostatic barrel 5, the second thermostatic barrel 6 and the third thermostatic barrel 7, and fixed plates 23 mounted on the two side walls of the first thermostatic barrel 5, the second thermostatic barrel 6 and the third thermostatic barrel 7. The movable feed plate 9 is composed of two symmetrically connected semi-conical hollow circular tubes. The upper ends of the two semi-ring plates 8 are fixed with sleeves 14, and the sleeves 14 are slidably sleeved on the corresponding limit rods 13. The two ends of the limit rod 13 are respectively fixedly connected to the two fixed plates 23;

[0071] A slide plate 10 slidably connected to the corresponding fixed plate 23 is fixed on each of the two half-ring plates 8, and a first mounting block with an inclined surface is provided on both side ends of the slide plate 10, and a plurality of second mounting blocks with inclined surfaces are provided in a straight line on the fixed plate 23 and on both sides of the slide plate 10, the inclined surface of the first mounting block is opposite to and parallel to the inclined surface of the second mounting block, a first permanent magnet is provided on the inclined surface of the first mounting block, and a second permanent magnet is provided on the inclined surface of the second mounting block, and the first permanent magnet 11 and the second permanent magnet 12 have the same magnetic poles at opposite ends;

[0072] An upper conical guide portion 42 and a lower conical guide portion 41 are respectively provided at the upper and lower ends of the material storage barrel 4 , and a plurality of material feeding openings 43 are provided on the upper conical guide portion 42 .

[0073] When the storage barrel 4 is transported to the constant temperature barrel by the driving cylinder 3, as the storage barrel 4 descends, the lower conical guide portion 41 at the lower end of the storage barrel 4 contacts and squeezes the upper inner inclined surface of the movable feed plate 5, and finally causes the two relatively arranged movable feed plates 9 to move in opposite directions. At this time, the semi-annular plate 8 will move along the fixed plate 23 through the slide plate 10. During the movement, the repulsive force generated between the second permanent magnet 12 and the first permanent magnet 11 will be overcome. This repulsive force is a resistance. When the storage barrel 4 is completely moved into the constant temperature barrel, the repulsive force generated between the second permanent magnet 12 and the first permanent magnet 11 will push the semi-annular plate 8 to move in the opposite direction (the repulsive force is an assist force at this time), that is, the two semi-annular plates 8 drive the two movable feed plates 9 to move together, and finally return to their original position, thereby achieving sealing of the upper end of the constant temperature barrel (at this time, the output end of the movable cylinder is located in the cavity surrounded by the two movable feed plates 9);

[0074] When the storage barrel 4 is moved out of the thermostatic barrel by the driving cylinder 3, as the storage barrel 4 moves upward, the upper conical guide portion 42 at its upper end contacts and squeezes the lower inner slope of the movable feed plate 9, and finally causes the two relatively arranged movable feed plates 9 to move in opposite directions. After the storage barrel 4 is moved out of the thermostatic barrel, the repulsive force generated between the second permanent magnet 12 and the first permanent magnet 11 pushes the semi-annular plate 8 to move in the opposite direction, and finally restores the semi-annular plate 8 and the movable feed plate 9 to their original positions.

[0075] The cooperation of the semi-ring plate 8 and the movable feed plate 9 automatically shields the upper end of the thermostatic barrel, which can effectively prevent excessive heat exchange between the internal thermostatic water and the outside air, thereby helping to maintain a stable internal temperature in the thermostatic barrel while avoiding an increase in the power consumption of the container.

[0076] It should be noted that: 1. The second permanent magnet 12 and the first permanent magnet 11 are arranged obliquely and parallel to each other, so that there is always a repulsive force pushing the two movable feed plates 9 to move together; 2. The semi-annular plate 8 and the movable feed plate 9 are both made of thermal insulation material; 3. The structures of the three constant temperature barrels are consistent.

[0077] As a preferred implementation mode in this embodiment, it also includes a second sealing unit, which automatically seals or releases the seal of the cavity formed between the two movable feed plates 9 without affecting the movement of the storage barrel 4 in and out of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7.

[0078] Since there is a cavity between the two contacting movable feed plates that allows the output end of the driving cylinder 3 to pass through, after the storage barrel 4 moves out of the constant temperature barrel and before the next storage barrel 4 enters this constant temperature barrel, the outside air can easily pass through this cavity to exchange heat with the constant temperature water in the constant temperature barrel. Therefore, a second sealing unit is provided to automatically seal this cavity to further prevent heat exchange.

[0079] As a preferred implementation in this embodiment, Figure 4 and Figure 5 As shown, the second sealing unit includes an upper blocking plate 15 and a lower bottom plate 17 with water flow holes connected together by a connecting rod 16, and T-shaped rods 18 slidably connected to the corresponding inner walls of the thermostatic barrel are fixed on both side walls of the lower bottom plate 17;

[0080] Two mounting frames for guide wheel groups 19 are symmetrically arranged on the outer wall of the thermostatic barrel, and both guide wheel groups 19 are equipped with pull ropes 21, and one end of the two pull ropes 12 is connected to the corresponding T-shaped rods 18 respectively, and the other end of the two pull ropes 21 is connected to the weight 22.

[0081] At the beginning, the upper blocking plate 15 blocks the cavity to form a seal. When the storage barrel 4 enters the thermostatic barrel, its two movable feed plates 9 move downward under the pressure of the inner lower conical guide part 41, and finally make the lower end of the storage barrel 4 contact and squeeze the upper end of the upper blocking plate 15. As the storage barrel 4 continues to move downward, the upper blocking plate 15 will overcome the gravity of the weight 22 and move downward, and finally make the lower bottom plate 17 contact with the bottom of the inner cavity of the thermostatic barrel;

[0082] When the material storage barrel 4 moves upward and moves out of the constant temperature barrel, the upper blocking plate 15 moves upward by the gravity of the two weights 22 and finally blocks the cavity;

[0083] The cavity can be blocked automatically without hindering the storage barrel from entering or exiting the constant temperature barrel.

[0084] As a preferred implementation in this embodiment, the diameter of the smallest circular cavity formed between the two movable feed plates 9 is consistent with the diameter of the output end of the driving cylinder 3 .

[0085] When the cavity diameter is consistent with the output shaft diameter of the drive cylinder 3, the semi-ring plate 8 and the two movable feed plates 9 can form a complete seal for the constant temperature barrel, which can effectively prevent external air from entering the constant temperature barrel 1 through the gap between the cavity and the output shaft of the drive cylinder 3 for heat exchange.

[0086] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing sodium fluorosilicate using waste acid from copper smelting and arsenic removal and an aging container, characterized in that: The steps include: S1: filtering the fluorine-containing waste acid after arsenic removal and placing it in a reaction tank 1, wherein the filtration is to remove solid particles and impurities in the waste acid; S2: Add silicon dioxide, heat and stir to react for 0.5 to 1 hour, convert the fluoride in the waste acid to produce fluorosilicic acid, and filter the reaction product; S3: transporting the generated fluorosilicic acid to the second reaction tank, adding an appropriate amount of saturated sodium sulfate liquid to prepare sodium fluorosilicate; S4: aging treatment, the product in the reaction tank 2 in step S3 is transported to an aging container for aging treatment, and filtered after aging. The temperature during aging is controlled at 25°C-65°C. The temperature control is divided into three stages. The aging time is 4 to 6 hours, and stirring is performed every 0.5 hours. The temperature control includes the following stages; S41: In the first temperature control stage, the temperature is controlled at 25°C-30°C for 1 to 2 hours; S42: The second temperature control stage, the temperature is controlled at 45°C-50°C, and the duration is 1 to 2 hours; S43: The third temperature control stage, the temperature is controlled at 60℃-65℃; the duration is 1 to 2 hours; S5: washing and drying the produced sodium fluorosilicate precipitate to obtain a final product.

2. An aging container, used in the method for preparing sodium fluorosilicate using waste acid from copper smelting and arsenic removal as claimed in claim 1, characterized in that: It comprises an O-shaped electric track 1 on which a plurality of electric sliders 2 are arranged, each of the plurality of electric sliders 2 is provided with a driving cylinder 3, and each of the output ends of the driving cylinders 3 is provided with a material storage barrel 4, and three groups of thermostatic barrels are arranged in sequence below the material storage barrel 4, namely a first thermostatic barrel 5, a second thermostatic barrel 6 and a third thermostatic barrel 7; The inner cavity of the storage barrel 4 is provided with a stirring shaft 44 driven by a motor, and the lower end of the storage barrel 4 is provided with a liquid outlet pipe 45 with an electric valve; The upper ends of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7 are all open, the first constant temperature barrel 5 is connected to the chiller through a connecting pipe, and the inner walls of the second constant temperature barrel 6 and the third constant temperature barrel 7 are provided with electric heating pipes, and the motor, the electric valve, the chiller, the electric heating pipe, the drive cylinder 3 and the O-shaped electric track 1 are all electrically connected to the PLC controller.

3. An aging container according to claim 2, characterized in that: It also includes a first sealing unit for sealing the openings of the three groups of constant temperature barrels, and automatically releasing the cover of the openings or automatically covering the openings when the storage barrel 4 enters or moves out of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7.

4. An aging container according to claim 3, characterized in that: The first sealing unit includes two movable feed plates 9 respectively mounted on the corresponding semi-ring plates 8 of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7, and fixed plates 23 mounted on the two side walls of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7, the movable feed plate 9 is composed of two symmetrically connected semi-conical hollow circular tubes, the upper ends of the two semi-ring plates 8 are fixed with sleeves 14, and the sleeves 14 are slidably sleeved on the corresponding limit rods 13, and the two ends of the limit rods 13 are respectively fixedly connected to the two fixed plates 23; A slide plate 10 slidably connected to the corresponding fixed plate 23 is fixed on each of the two semi-ring plates 8, and a first mounting block with an inclined surface is provided on both side ends of the slide plate 10, and a plurality of second mounting blocks with inclined surfaces are provided in a straight line on the fixed plate 23 and on both sides of the slide plate 10, the inclined surface of the first mounting block is opposite to and parallel to the inclined surface of the second mounting block, a first permanent magnet 11 is provided on the inclined surface of the first mounting block, and a second permanent magnet 12 is provided on the inclined surface of the second mounting block, and the first permanent magnet 11 and the second permanent magnet 12 have the same magnetic poles at opposite ends; An upper conical guide portion 42 and a lower conical guide portion 41 are respectively provided at the upper and lower ends of the material storage barrel 4 , and a plurality of material feeding openings 43 are provided on the upper conical guide portion 42 .

5. An aging container according to claim 4, characterized in that: It also includes a second sealing unit, which automatically seals or releases the seal of the cavity formed between the two movable feed plates 9 without affecting the movement of the storage barrel 4 in and out of the first constant temperature barrel 5, the second constant temperature barrel 6 and the third constant temperature barrel 7.

6. An aging container according to claim 5, characterized in that: The second sealing unit includes an upper blocking plate 15 and a lower bottom plate 17 with water flow holes connected together by a connecting rod 16, and T-shaped rods 18 slidably connected to the corresponding inner walls of the thermostatic barrel are fixed on both side walls of the lower bottom plate 17; Two mounting frames 20 for guide wheel groups 19 are symmetrically arranged on the outer wall of the thermostatic barrel, and both guide wheel groups 19 are equipped with pull ropes 21, and one end of the two pull ropes 21 is connected to the corresponding T-shaped rods 18 respectively, and the other end of the two pull ropes 21 is connected to the weight 22.

7. An aging container according to claim 4, characterized in that: The diameter of the smallest circular cavity formed between the two movable feed plates 9 is consistent with the diameter of the output end of the driving cylinder 3 .

Citation Information

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