Process for producing ammonium paratungstate by treating wolframite with sulfuric acid
Through the innovative design of the drying bucket and airbag ring structure, combined with crystal sliding and flip, the problems of low efficiency and high energy consumption in the drying process of the production of ammonium paratungsten ore in sulfuric acid treatment, achieving efficient continuous processing and stability of product quality.
Patent Information
- Application Number
- CN202510653975.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-21
- Publication Date
- 2025-08-15
AI Technical Summary
In the existing process of producing ammonium paratungstate in sulfuric acid treatment, the crystal drying process is low, the energy consumption is high, and the product quality is unstable, especially the drying time is too long that affects the production efficiency.
The drying bucket and airbag ring structure in the drying device are adopted, combining the sliding and flip of the crystal, the crystal flow rate is adjusted by controlling the expansion degree of the airbag ring, and the movement of the drying bucket is used to accelerate the crystal sliding speed, and the feed and discharge structures are set to achieve continuous processing.
The drying efficiency of ammonium paratungstate is improved, residues and clogs are avoided, continuous processing is achieved, and production efficiency and product quality stability are improved.
Smart Images
Figure CN120483255A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of ammonium paratungstate production, and in particular to a process for producing ammonium paratungstate by treating wolframite with sulfuric acid. Background Art
[0002] Ammonium paratungstate (APT) is an important tungsten compound widely used in cemented carbide and tungsten powder production. Traditionally, APT production involves treating wolframite with sulfuric acid. However, the drying process for APT crystals has been plagued by low efficiency, high energy consumption, and inconsistent product quality.
[0003] In the existing process of producing ammonium paratungstate by treating wolframite with sulfuric acid, the separated ammonium paratungstate crystals are usually placed in a drying tray and dried in a hot air drying oven or a hot air circulation oven for 4 to 8 hours. The drying time is relatively long, which affects the production efficiency of ammonium paratungstate.
[0004] Therefore, it is necessary to propose a process for producing ammonium paratungstate by treating wolframite with sulfuric acid to solve the above problems. Summary of the Invention
[0005] The present invention aims to provide a process for producing ammonium paratungstate by treating wolframite with sulfuric acid, so as to solve the problem that in the existing process for producing ammonium paratungstate by treating wolframite with sulfuric acid, the separated ammonium paratungstate crystals are usually placed in a drying tray and dried in a hot air drying oven or a hot air circulation oven for 4 to 8 hours, which lasts for a long time and affects the production efficiency of the ammonium paratungstate.
[0006] To achieve the above object, the present invention provides the following technical solution: a process for producing ammonium paratungstate by treating wolframite with sulfuric acid, comprising the following steps:
[0007] S1, impurity removal, pre-treating the wolframite to remove impurities;
[0008] S2, reacting the pretreated wolframite with sulfuric acid to generate a sulfuric acid tungstic acid solution;
[0009] S3, purification, purifying the sulfuric acid tungstic acid solution to remove impurity ions;
[0010] S4, crystallization, evaporating and crystallizing the purified tungstic acid sulfate solution to obtain ammonium paratungstate crystals;
[0011] S5, drying, using a drying device to dry the ammonium paratungstate crystals to obtain an ammonium paratungstate product;
[0012] The drying device includes a drying cylinder and a drying hopper arranged inside the drying cylinder. The drying hopper is truncated and has a small inner diameter at the end close to the feed. An air bag ring is arranged on the inner wall of the drying hopper to control the crystal flow rate.
[0013] Preferably, a fixing ring is fixedly connected to the inner wall of the drying cylinder, a sliding sleeve is slidably provided inside the fixing ring, and the drying hopper is fixedly connected to the inner ring of the sliding sleeve.
[0014] Preferably, a second support block is fixedly connected to the sliding sleeve, an air cylinder is fixedly connected to the fixed ring, a sliding column is slidingly provided inside the air cylinder, an end of the sliding column away from the air cylinder is fixedly connected to the second support block, an air box is fixedly connected to the outer wall of the drying hopper, the air box cooperates with the airbag ring, and the air box cooperates with the air cylinder through a connecting component.
[0015] Preferably, the airbag rings are provided in plurality, and the plurality of airbag rings are distributed at equal distances.
[0016] Preferably, a control assembly for controlling the movement of the drying hopper is provided between the fixing ring, and the control assembly includes an electric push rod and a first support block.
[0017] Preferably, a frame is provided on the outside of the drying cylinder, and the drying cylinder is rotatably provided on the frame. A feed cylinder is provided at one end of the frame, and a discharge cylinder is provided at one end of the frame, and the feed cylinder is close to the end with the smaller inner diameter of the drying hopper, and the feed cylinder and the discharge cylinder are both coordinated with the drying cylinder.
[0018] Preferably, an equipment box is installed at the feed barrel, and a blower fan and a heating device are installed inside the equipment box.
[0019] Preferably, an exhaust fan is installed at the discharge barrel.
[0020] Preferably, a filter plate is fixedly connected to the inner wall of the discharge barrel, and the bottom end of the discharge barrel is connected to a discharge hopper.
[0021] Preferably, the top of the feed barrel is connected to a feed hopper, an air bag is fixedly connected to the inner wall of the feed hopper, and a pump body that cooperates with the air bag is provided on the outside of the feed barrel.
[0022] The technical effects and advantages of the present invention are as follows:
[0023] 1. The present invention combines the sliding and flipping of the crystals by providing structures such as a drying hopper and an air bag ring, thereby improving the drying efficiency. The expansion degree of the air bag ring is used to control the flow rate of the crystals, thereby improving the efficiency of the process for producing ammonium paratungstate by treating wolframite with sulfuric acid.
[0024] 2. The present invention drives the drying hopper to move back and forth by arranging the drying hopper, the air cylinder and the control assembly, which can also speed up the sliding speed of the crystals and avoid the residue in the drying hopper;
[0025] 3. Set up the feed hopper, discharge barrel and other structures, feed the material into the feed hopper, dry it in the drying hopper, and then discharge it from the discharge barrel, so as to achieve the purpose of continuous processing;
[0026] 4. The present invention provides a guide frame, a vertical rod and other structures, and uses the movement of the drying hopper to hit the vertical rod, causing the guide frame to vibrate, thereby avoiding residue, blockage and the like on the guide frame;
[0027] 5. The airbag switches between expansion and contraction, producing a shaking effect to prevent blockage inside the feed hopper. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 This is a process flow chart of producing ammonium paratungstate by treating wolframite with sulfuric acid according to the present invention.
[0029] Figure 2 It is a schematic structural diagram of the drying equipment of the present invention.
[0030] Figure 3 For the present invention Figure 2 A magnified schematic diagram of the structure in the middle.
[0031] Figure 4 It is a schematic cross-sectional structural diagram of the drying equipment of the present invention.
[0032] Figure 5 For the present invention Figure 4 A magnified schematic diagram of the structure at point B in the middle.
[0033] Figure 6 For the present invention Figure 4 Enlarged schematic diagram of the structure at point C in the middle.
[0034] Figure 7 For the present invention Figure 6 Enlarged schematic diagram of the structure at point D in the middle.
[0035] In the figure: 1. Frame; 2. Drying cylinder; 3. Feed cylinder; 4. Discharge cylinder; 5. Discharge hopper; 6. Fixed ring; 7. Drying hopper; 8. Slide; 9. Electric push rod; 10. First support block; 11. Air bag ring; 12. Second support block; 13. Slide column; 14. Air cylinder; 15. Air pipe; 16. Air box; 17. First air hole; 18. Second air hole; 19. Filter plate; 20. Supply fan; 21. Heating device; 22. Exhaust fan; 23. Feed hopper; 24. Air bag; 25. Pump body; 26. Drive device; 27. Equipment box; 28. Guide frame; 29. Vertical rod. DETAILED DESCRIPTION
[0036] The present invention provides Figures 1 to 7 The process for producing ammonium paratungstate by treating wolframite with sulfuric acid shown in the figure includes the following steps:
[0037] S1, impurity removal, pre-treating the wolframite to remove impurities;
[0038] S2, reacting the pretreated wolframite with sulfuric acid to generate a sulfuric acid tungstic acid solution;
[0039] S3, purification, purifying the sulfuric acid tungstic acid solution to remove impurity ions;
[0040] S4, crystallization, evaporating and crystallizing the purified tungstic acid sulfate solution to obtain ammonium paratungstate crystals;
[0041] S5, drying, using a drying device to dry the ammonium paratungstate crystals to obtain an ammonium paratungstate product;
[0042] Reference Figure 2 、 Figure 4 As shown in the figure, the drying device includes a drying cylinder 2 and a drying hopper 7 arranged inside the drying cylinder 2. A frame 1 is provided on the outside of the drying cylinder 2, and the drying cylinder 2 is rotatably arranged on the frame 1. A feed cylinder 3 is fixedly provided at one end of the frame 1, and a discharge cylinder 4 is fixedly provided at one end of the frame 1. The feed cylinder 3 and the discharge cylinder 4 are both connected and cooperated with the drying cylinder 2.
[0043] A driving device 26 for driving the drying cylinder 2 to rotate is provided between the drying cylinder 2 and the frame 1. The driving device 26 includes a motor, gears and other structures. The driving device 26 is a common existing technology and will not be described in detail here.
[0044] The feeding cylinder 3 is provided with an equipment box 27, and a blower fan 20 and a heating device 21 are installed inside the equipment box 27, and the heating device 21 is located at one end of the equipment box 27 close to the drying cylinder 2 (refer to FIG. Figure 4 ), the heating device 21 includes structures such as electric heating wires, which can quickly heat the gas passing through the equipment box 27. The heating device 21 is a common existing technology and will not be described in detail here.
[0045] An exhaust fan 22 is installed at the discharge barrel 4, and the supply fan 20, the heating device 21 and the exhaust fan 22 are all connected to the factory circuit for power supply.
[0046] When the supply fan 20 is running, the external air is sucked into the equipment box 27, and is heated by the heating device 21 and then transported to the inside of the drying hopper 7. At the same time, the exhaust fan 22 sucks the inside of the drying hopper 7, thereby forming a dry airflow inside the drying hopper 7 to dry the crystals.
[0047] A filtering device (not shown in the figure) is provided at one end of the supply fan 20 away from the drying cylinder 2. The filtering device includes a filter screen and other structures to prevent impurities from entering the interior of the drying cylinder 2. At the same time, the factory's air treatment duct is connected to the exhaust fan 22 to process the exhausted gas, which can be adjusted according to specific usage conditions.
[0048] Reference Figure 4 As shown in the figure, the drying hopper 7 is truncated, with a smaller inner diameter at the end closest to the feed cylinder 3. As the drying hopper 7 rotates, the crystals tumble, drying them evenly. Simultaneously, the crystals slide along the inclined surface of the drying hopper's inner wall toward the discharge cylinder 4. Furthermore, in actual use, the drying hopper 7 is provided with micropores (not shown) to improve drying efficiency.
[0049] Reference Figure 4 As shown in FIG, a fixing ring 6 is fixedly connected to the inner wall of the drying cylinder 2, and a sliding sleeve 8 is slidably provided inside the fixing ring 6. A drying hopper 7 is fixedly connected to the inner ring of the sliding sleeve 8. Specifically, when the drying cylinder 2 rotates, the fixing ring 6 and sliding sleeve 8 drive the drying hopper 7 to rotate synchronously, causing the crystals to tumble and improve the drying effect. At the same time, the crystals can slide along the inclined surface of the inner wall of the drying hopper 7 toward the discharge cylinder 4, achieving automatic discharge.
[0050] Reference Figure 4 As shown in FIG, to control the flow rate of the crystals within the drying hopper 7, an airbag ring 11 is provided on the inner wall of the drying hopper 7 to control the crystal flow rate. When the airbag ring 11 expands, it forms a barrier on the inner wall of the drying hopper 7, reducing the crystal flow rate. The greater the expansion of the airbag ring 11, the more significant the barrier effect, which can extend the crystal drying time. When the airbag ring 11 contracts, the barrier is released, allowing the crystals to flow normally.
[0051] The present invention combines the sliding and flipping of the crystals by providing structures such as the drying hopper 7 and the air bag ring 11, thereby improving the drying efficiency. The expansion degree of the air bag ring 11 is used to control the flow rate of the crystals, thereby improving the efficiency of the process of producing ammonium paratungstate by treating wolframite with sulfuric acid.
[0052] Furthermore, a plurality of airbag rings 11 are provided, and the plurality of airbag rings 11 are distributed at equal distances.
[0053] Reference Figure 4 As shown in, in order to achieve control of the expansion and contraction of the airbag ring 11, a second support block 12 is fixedly connected to the sliding sleeve 8, and an air cylinder 14 is fixedly connected to the fixed ring 6. A sliding column 13 is provided inside the air cylinder 14 for sliding, and one end of the sliding column 13 away from the air cylinder 14 is fixedly connected to the second support block 12; an air box 16 is fixedly connected to the outer wall of the drying bucket 7, and the air box 16 cooperates with the airbag ring 11. A second air hole 18 is provided on the side of the air box 16 close to the drying bucket 7. The air box 16 is communicated with the airbag ring 11 through the second air hole 18, and the air box 16 cooperates with the air cylinder 14 through a connecting component, which includes an air pipe 15 and a first air hole 17. One end of the air pipe 15 is fixedly connected to the air cylinder 14, and the other end of the air pipe 15 is fixedly connected to the air box 16. The first air hole 17 is opened on the air box 16, and the first air hole 17 is distributed correspondingly to the air pipe 15. The air cylinder 14 is communicated with the air box 16 via the air pipe 15 and the first air hole 17.
[0054] A control component for controlling the movement of the drying hopper 7 is provided between the fixed ring 6, and the control component includes an electric push rod 9 and a first support block 10. The first support block 10 is fixedly connected to the outer wall of the sliding sleeve 8, the electric push rod 9 is fixedly connected to the fixed ring 6, and the first support block 10 is fixedly connected to the telescopic end of the electric push rod 9.
[0055] Reference Figure 4 、 Figure 6 、 Figure 7 As shown in , in actual use, the telescopic end of the electric push rod 9 is controlled to extend, and the drying bucket 7 is driven to move to the right through the sliding sleeve 8. At this time, the slide column 13 moves to the right synchronously, and the air cylinder 14 uses the air pipe 15, the first air hole 17, the air box 16 and the second air hole 18 to suck the gas inside the airbag ring 11, so that the airbag ring 11 shrinks; the telescopic end of the electric push rod 9 is controlled to retract, and the drying bucket 7 is driven to move to the left through the sliding sleeve 8. At this time, the slide column 13 moves to the left synchronously, and the gas inside the air cylinder 14 enters the interior of the airbag ring 11 through the air pipe 15, the first air hole 17, the air box 16 and the second air hole 18, and the airbag ring 11 expands.
[0056] In addition, a power supply device is provided on the fixing ring 6 to supply power to the electric push rod 9. The power supply device includes a battery and other structures. The power supply device is a common existing technology and will not be described in detail here.
[0057] The drying bucket 7 moves back and forth, which can also speed up the sliding speed of the crystals. For example, when a small amount of crystals remain at a certain air bag ring 11, the drying bucket 7 can be moved back and forth.
[0058] The present invention drives the drying hopper 7 to move back and forth by arranging the drying hopper 7 , the air cylinder 14 and the control assembly, which can also speed up the sliding speed of the crystal and avoid the residue in the drying hopper 7 .
[0059] Reference Figure 4 As shown in the figure, a filter plate 19 is fixedly connected to the inner wall of the discharge barrel 4. The filter plate 19 is provided to prevent the exhaust fan 22 from directly extracting the crystals. The bottom end of the discharge barrel 4 is connected to a discharge hopper 5 for discharging the dried crystals, and a collection container is provided below the discharge hopper 5 for collecting the dried crystals.
[0060] The top of the feed cylinder 3 is connected to the feed hopper 23, and the bottom end of the feed hopper 23 is installed with a guide frame 28, and the bottom end of the guide frame 28 extends into the interior of the drying hopper 7. The bottom of the guide frame 28 is fixedly connected to a vertical rod 29. The feed hopper 23 is used for loading, and the feed hopper 23 and the guide frame 28 enter the interior of the drying hopper 7; when the drying hopper 7 moves toward the feed cylinder 3 and hits the vertical rod 29, the guide frame 28 will shake to avoid residue, blockage, etc. at the guide frame 28.
[0061] In addition, a feed hopper 23, a discharge cylinder 4 and other structures are provided. The feed hopper 23 is used to feed the material, the material is dried in the drying hopper 7, and then the material is discharged from the discharge cylinder 4, thereby achieving the purpose of continuous processing.
[0062] The present invention provides a guide frame 28, a vertical rod 29 and other structures, and utilizes the movement of the drying hopper 7 to hit the vertical rod 29, causing the guide frame 28 to vibrate, thereby avoiding residue, blockage and the like at the guide frame 28.
[0063] In order to prevent blockage in the feed hopper 23, an air bag 24 is fixedly connected to the inner wall of the feed hopper 23, and a pump body 25 cooperating with the air bag 24 is provided on the outside of the feed tube 3, and the pump body 25 can switch between suction and air supply. When gas is transported to the inside of the air bag 24, the air bag 24 expands and becomes larger. When the inside of the air bag 24 is sucked, the air bag 24 shrinks and becomes smaller. The air bag 24 switches between expansion and contraction, producing a shaking effect to prevent blockage in the feed hopper 23; and the degree of expansion of the air bag 24 can control the degree of opening and closing of the inside of the feed hopper 23, thereby controlling the instantaneous feed amount.
[0064] Working principle: The material is loaded into the feed hopper 23 and enters the interior of the drying hopper 7 through the feed hopper 23 and the guide frame 28; when the drying hopper 7 moves toward the feed cylinder 3 and hits the vertical rod 29, the guide frame 28 will shake to avoid residue, blockage, etc.
[0065] During actual use, the telescopic end of the electric push rod 9 is controlled to extend, and the drying bucket 7 is driven to move to the right through the sliding sleeve 8. At this time, the slide column 13 moves to the right synchronously, and the air cylinder 14 uses the air pipe 15, the first air hole 17, the air box 16 and the second air hole 18 to suck the gas inside the airbag ring 11, so that the airbag ring 11 shrinks; the telescopic end of the electric push rod 9 is controlled to retract, and the drying bucket 7 is driven to move to the left through the sliding sleeve 8. At this time, the slide column 13 moves to the left synchronously, and the gas inside the air cylinder 14 enters the interior of the airbag ring 11 through the air pipe 15, the first air hole 17, the air box 16 and the second air hole 18, and the airbag ring 11 expands.
[0066] When the drying cylinder 2 rotates, the drying hopper 7 will be driven to rotate synchronously through the fixed ring 6 and the sliding sleeve 8, and the crystals will roll, thereby improving the drying effect; at the same time, the crystals can slide along the inclined surface of the inner wall of the drying hopper 7 toward the discharge cylinder 4, realizing automatic discharge.
Claims
1. A process for producing ammonium paratungstate by treating wolframite with sulfuric acid, characterized by: The following steps are included: S1, impurity removal, pre-treating the wolframite to remove impurities; S2, reacting the pretreated wolframite with sulfuric acid to generate a sulfuric acid tungstic acid solution; S3, purification, purifying the sulfuric acid tungstic acid solution to remove impurity ions; S4, crystallization, evaporating and crystallizing the purified tungstic acid sulfate solution to obtain ammonium paratungstate crystals; S5, drying, using a drying device to dry the ammonium paratungstate crystals to obtain an ammonium paratungstate product; The drying device comprises a drying cylinder (2) and a drying hopper (7) arranged inside the drying cylinder (2). The drying hopper (7) is in a truncated cone shape and has a smaller inner diameter at the end close to the feed. An air bag ring (11) for controlling the crystal flow rate is arranged on the inner wall of the drying hopper (7).
2. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 1, characterized in that: A fixing ring (6) is fixedly connected to the inner wall of the drying cylinder (2), a sliding sleeve (8) is slidably provided inside the fixing ring (6), and the drying hopper (7) is fixedly connected to the inner ring of the sliding sleeve (8).
3. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 2, characterized in that: The sliding sleeve (8) is fixedly connected to a second support block (12), the fixed ring (6) is fixedly connected to an air cylinder (14), a sliding column (13) is slidably provided inside the air cylinder (14), and one end of the sliding column (13) away from the air cylinder (14) is fixedly connected to the second support block (12), and an air box (16) is fixedly connected to the outer wall of the drying hopper (7), the air box (16) cooperates with the air bag ring (11), and the air box (16) cooperates with the air cylinder (14) through a connecting component.
4. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 1, characterized in that: The airbag rings (11) are provided in plurality, and the plurality of airbag rings (11) are distributed at equal distances.
5. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 1, characterized in that: A control assembly for controlling the movement of the drying hopper (7) is provided between the fixing ring (6), and the control assembly comprises an electric push rod (9) and a first support block (10).
6. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 1, characterized in that: A frame (1) is provided on the outside of the drying cylinder (2), and the drying cylinder (2) is rotatably provided on the frame (1). A feed cylinder (3) is provided at one end of the frame (1), and a discharge cylinder (4) is provided at one end of the frame (1). The feed cylinder (3) is close to the end of the drying hopper (7) with a smaller inner diameter, and both the feed cylinder (3) and the discharge cylinder (4) cooperate with the drying cylinder (2).
7. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 6, characterized in that: An equipment box (27) is installed at the feeding barrel (3), and a blower fan (20) and a heating device (21) are installed inside the equipment box (27).
8. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 6, characterized in that: An exhaust fan (22) is installed at the discharge barrel (4).
9. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 6, characterized in that: A filter plate (19) is fixedly connected to the inner wall of the discharge barrel (4), and the bottom end of the discharge barrel (4) is connected to a discharge hopper (5).
10. The process for producing ammonium paratungstate by treating wolframite with sulfuric acid according to claim 6, characterized in that: The top of the feed barrel (3) is connected to a feed hopper (23), an air bag (24) is fixedly connected to the inner wall of the feed hopper (23), and a pump body (25) matched with the air bag (24) is provided on the outside of the feed barrel (3).