An integrated precipitation and calcination apparatus and method
By designing an integrated precipitation and calcination device, the precipitation and calcination processes are integrated. Electromagnetic pumps, liquid inlet pipes, centrifuges, and robotic arms are used to achieve uniform dispensing and calcination of the precipitated slurry. This solves the equipment stability and efficiency problems caused by the independent operation of precipitation and calcination in the existing technology, and realizes efficient integrated operation.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-23
- Publication Date
- 2026-03-06
AI Technical Summary
In existing technologies, precipitation and calcination are two separate operating units, which makes the process less compact, requires multiple vessels, is not suitable for fine chemicals, and has issues with equipment stability and efficiency.
Design an integrated precipitation and calcination device that integrates precipitation and calcination processes. Employ an electromagnetic pump, liquid inlet pipe, precipitant tank, centrifuge, precipitation reactor, high-level storage tank, calcination furnace, and robotic arm. Through remote control and programmed operation, the device achieves uniform dispensing of the precipitated slurry, solid-liquid separation, and calcination. The robotic arm and vacuum pump are used for material transfer and heating.
It achieves efficient integrated operation of precipitation and calcination, reduces material loss, improves equipment stability and processing efficiency, reduces system retention, and is suitable for scenarios with large batch processing volumes.
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Figure CN116272004B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of chemical solution precipitation and crystallization equipment and precipitate drying and calcination equipment, specifically relating to an integrated precipitation and calcination device and a precipitation and calcination method. Background Technology
[0002] Precipitation and crystallization is a common unit operation in the chemical industry, widely used in metallurgy, mining, and water treatment. This unit operation can purify liquid feed and convert elements from liquid to solid, followed by solid-liquid separation via filtration. In industrial operations, solution precipitation and crystallization are often carried out in batches using reaction vessels, and the precipitate needs to be transferred out for filtration after the precipitation and crystallization process. However, for precipitation and crystallization operations with large batch throughput, if the precipitate slurry cannot be transferred out evenly from batch to batch, it can easily cause fluctuations in the feed conditions of subsequent processes, adversely affecting equipment stability.
[0003] Calcination is a fundamental operational unit in chemical processing, involving several physicochemical processes such as thermal decomposition and recrystallization. It is widely used in industries such as mining, metallurgy, building materials, and chemicals. By appropriately controlling the calcination temperature, chemically free and bound water can be removed, and specific crystal forms, crystal sizes, specific surface areas, and pore structures can be obtained through calcination. In industrial production, the solid material separated from the liquid phase is typically placed in a specialized container and then fed into a calcination furnace to complete the calcination process.
[0004] Currently, precipitation and calcination are two separate operation units. After precipitation, solid-liquid separation is carried out, and the separated solid material is transferred to the calcination process to complete the calcination. The process is not compact enough, requires a lot of equipment, and has a large loss, making it unsuitable for fine chemical industry applications.
[0005] In view of the shortcomings of the existing technology, there is an urgent need to design a simple and efficient integrated precipitation and calcination device and precipitation and calcination method. Summary of the Invention
[0006] The purpose of this invention is to provide an integrated precipitation and calcination device and method that integrates precipitation and calcination, achieving simplicity and high efficiency.
[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:
[0008] An integrated precipitation and calcination apparatus includes an electromagnetic pump, an inlet pipe, a precipitant tank, an external frame, a mother liquor storage tank, a centrifuge, a precipitation reactor, an elevated storage tank, a calcination furnace, and a robotic arm. The precipitant tank is located at the lower part of the external frame, while the centrifuge, precipitation reactor, elevated storage tank, calcination furnace, and robotic arm are located at the upper part of the external frame. The inlet pipe runs through the precipitation reactor and the elevated storage tank. The electromagnetic pump transports the precipitant stock solution and precipitant from the precipitant tank to the elevated storage tank via the inlet pipe, then into the precipitation reactor, and finally into the mother liquor storage tank located inside the centrifuge through the outlet of the precipitation reactor. The robotic arm transfers the material between the calcination furnace and the centrifuge.
[0009] Furthermore, a ring-shaped centrifuge rack is installed below the outlet of the precipitation reactor, and six material cups are placed on the ring-shaped centrifuge rack, which can be removed.
[0010] The integrated precipitation and calcination device is also equipped with remote operation functionality. Operators can send action commands via a central control console, and the robotic arm will execute the predetermined actions upon receiving the signal. Through remote control and program writing, each material cup is automatically rotated and positioned at the lower end of the discharge port. The rotation actuator is located inside the centrifuge, driving the rotation of the annular centrifuge frame, and the material cups are placed on the annular frame.
[0011] Mother liquor storage tanks are mainly used to store precipitating stock solution, precipitant, and washing liquid.
[0012] The calcining furnace includes a base and a bell-shaped furnace lid. A material cup rack is installed on the base; this hollow rack can hold six material cups at a time and is mainly used to fix the material cups and position the robotic arm. A liftable insulation cover is installed above the material cup rack. After the calcining furnace is closed, the insulation cover is fastened to the material rack to prevent the insulation layer inside the calcining furnace from falling off and contaminating the material.
[0013] The precipitation reactor is equipped with an automatic weighing device. After cleaning at the end of each reaction, the automatic weighing device is automatically zeroed through a logic algorithm.
[0014] A valve assembly is installed at the lower end of the discharge port of the sedimentation reactor, including a first valve and a second valve, which are a pneumatic valve and a solenoid valve respectively, for discharging the sedimentation slurry. The valve assembly is a distributing device; the first valve is a gate valve, and the second valve is a butterfly valve. The mass of liquid dispensed each time is accurately measured by controlling the opening of the butterfly valve and the gate valve, as well as the automatic weighing device of the sedimentation reactor. The butterfly valve is a self-feedback regulating valve that automatically adjusts its opening based on the weight data fed back from the sedimentation reactor.
[0015] The equalization device quantitatively and evenly separates the precipitated slurry into 6 material cups; after the separation is completed, the centrifuge is turned on to complete the solid-liquid separation; the robotic arm will grab the material cups one by one and pour the supernatant into the mother liquor storage tank, controlling the pouring speed and the pouring angle of 8 degrees to ensure that the solid material flows out together; after the solid-liquid separation is completed, the robotic arm is remotely controlled to transfer the material cups one by one to the material cup rack of the calcining furnace; after the transfer is completed, the calcining furnace is turned off, the vacuum pump is turned on, and the heating temperature range is set to heat the material.
[0016] The top of the sedimentation reactor is sealed with a flange, and the flange has a through hole with a diameter larger than that of the inlet pipe. The bottom of the sedimentation reactor is constructed by welding an elliptical head. The sedimentation reactor is fixed by securing it to the edge of the top flange, without any hard connection to the inlet pipe, outlet, or other locations, thus avoiding stress concentration and breakage at pipe connections.
[0017] The centrifuge is located at the bottom of the sedimentation reactor, with the centrifuge rack positioned 3 cm below the discharge pipe. The rack has six cup openings. Uniform discharge and automatic rack rotation and positioning are achieved through program control. The centrifugation speed and time can be automatically and remotely set. The centrifuge rack and cup openings are connected flexibly. Under centrifugal force, the cup openings gradually tilt inwards, causing the heavy components (solid precipitates) to settle at the bottom of the cups, achieving solid-liquid separation.
[0018] The calcining furnace is equipped with a movement cylinder to raise and lower the furnace cover and insulation cover, and has remote control functionality. After the material transfer is completed, a furnace closing command is issued via the central control panel, which activates the furnace body lifting cylinder to slowly lower the furnace body. Once it reaches the designated position, the insulation layer automatically engages with the material rack, and the locking device and vacuum system are activated, completing the furnace closing process. After calcination is completed, a furnace opening command is issued via the central control panel. The vacuum stops, and the air supply vents slowly release pressure. Once the pressure returns to atmospheric pressure, the insulation cover automatically rises, the locking device opens, and the furnace body slowly rises, completing the furnace opening process.
[0019] Among them, the robotic arm is a five-axis robotic arm with high positioning accuracy and adjustable execution speed, which can smoothly complete actions such as pouring mother liquor, feeding precipitates, and discharging calcined materials.
[0020] The calcining furnace is an electric resistance furnace, used in conjunction with a vacuum pump, and has a bell-shaped exterior.
[0021] The integrated precipitation and calcination device is also equipped with a vacuum pump and a hydraulic column. The vacuum pump and hydraulic column are located at the lower part of the device's outer frame.
[0022] The outer edge of the integrated precipitation and calcination device is a sealing device that encloses the entire set of equipment to prevent material from polluting the environment.
[0023] The precipitation and calcination method using the above-mentioned integrated precipitation and calcination apparatus includes the following steps:
[0024] 1) Preparation before precipitation: After the stock solution and precipitant are prepared, they are stored in the precipitant tank. After the precipitation reaction vessel is emptied, the sensor reading of the automatic weighing device is cleared to zero by the logic controller.
[0025] 2) Precipitation Feeding: The precipitate stock solution is metered and added to the precipitation reactor through the feed pipe using an electromagnetic pump, and the stirrer is turned on. After the precipitate stock solution is added, the oxalic acid precipitant is metered and added to the precipitation reactor through the precipitant feed pipe using an electromagnetic pump. After the precipitant is added, the precipitate solution is aged.
[0026] 3) Slurry equalization: After aging, the number of slurry to be evenly divided is set to 6 in the logic controller. Automatic dispensing is started. The control system performs logical calculations based on the measurement values of the weighing device. After completion, automatic feeding is started. The logic controller automatically controls the ball valve to open to an appropriate degree based on the feedback signal to complete the slurry dispensing.
[0027] 4) Repeat step 3 until all 6 cups of precipitated slurry have been dispensed;
[0028] 5) Centrifugation: The precipitated material settles to the bottom of the cup under the action of centrifugal force;
[0029] 6) Calcination: After solid-liquid separation, the robotic arm places the gripping cup on the calcining furnace cup rack to begin calcination.
[0030] The beneficial effects achieved by this invention are as follows:
[0031] The integrated precipitation and calcination device provided by this invention is suitable for chemical precipitation and calcination processes, enabling integrated operation of liquid loading, precipitation, filtration, and calcination. Its design effectively utilizes space, minimizes excessively long process paths, reduces system retention in chemical processes, and improves batch processing capacity. It features high processing efficiency, low retention, high equipment integration, high sensitivity, and high automation, making it worthy of widespread application and minimizing material deposition and loss during the process. Attached Figure Description
[0032] Figure 1 This is a front view of the integrated precipitation and calcination unit;
[0033] Figure 2 This is a side view of the integrated precipitation and calcination unit.
[0034] In the diagram: 1. Precipitator tank; 2. Frame of the device; 3. Mother liquor storage tank; 4. Centrifuge; 5. Precipitation reactor; 6. High-level storage tank; 7. Insulation cover lifting mechanism; 8. Calcining furnace; 9. Hydraulic column; 10. Vacuum pump; 11. Enclosure device; 12. Robotic arm. Detailed Implementation
[0035] The present invention will now be described in detail with reference to specific embodiments.
[0036] like Figure 1 As shown, this invention provides an integrated precipitation and calcination apparatus, comprising an electromagnetic pump, an inlet pipe, a precipitant tank 1, an external frame 2, a mother liquor storage tank 3, a centrifuge 4, a precipitation reactor 5, an elevated storage tank 6, a calcination furnace 8, and a robotic arm 12. The precipitant tank 1 is located at the lower part of the external frame 2, while the centrifuge 4, precipitation reactor 5, elevated storage tank 6, calcination furnace 8, and robotic arm 12 are located at the upper part of the external frame 2. The inlet pipe passes through the precipitation reactor 5 and the elevated storage tank 6. The electromagnetic pump transports the precipitant stock solution and precipitant from the precipitant tank 1 to the elevated storage tank 6 via the inlet pipe, then into the precipitation reactor 5, and finally into the mother liquor storage tank 3 located inside the centrifuge 4 through the outlet of the precipitation reactor 5. The robotic arm 12 transfers the material between the calcination furnace 8 and the centrifuge 4.
[0037] Furthermore, a ring-shaped centrifuge rack is installed below the outlet of the precipitation reactor 5, and six material cups are installed on the ring-shaped centrifuge rack, which can be removed.
[0038] The integrated precipitation and calcination device is also equipped with a remote operation function. The operator sends action commands through the central control console, and the robotic arm 12 starts to execute the predetermined actions after receiving the signal. Through remote control and program writing, each material cup is controlled to automatically rotate and position itself at the lower end of the discharge port. The rotation actuator is located inside the centrifuge 4, driving the rotation of the annular centrifuge frame, and the material cup is placed on the annular material frame.
[0039] Mother liquor storage tank 3 is mainly used to store precipitate stock solution, precipitant and washing liquid.
[0040] The calcining furnace 8 includes a base and a bell-shaped furnace cover. A material cup rack is installed on the base, which is a hollow rack that can hold 6 material cups at a time. It is mainly used to fix the material cups and position the robotic arm 12. A liftable heat preservation cover is installed above the material cup rack. After the calcining furnace 8 is closed, the heat preservation cover is fastened to the material rack to prevent the heat preservation layer inside the calcining furnace from falling off and contaminating the material.
[0041] The precipitation reactor 5 is equipped with an automatic weighing device. After cleaning at the end of one reaction, the automatic weighing device is automatically zeroed through a logic algorithm.
[0042] A valve assembly is installed at the lower end of the discharge port of the sedimentation reactor 5, including a first valve and a second valve, which are a pneumatic valve and a solenoid valve respectively, for discharging the sedimentation slurry. The valve assembly is a distributing device; the first valve is a gate valve, and the second valve is a butterfly valve. The mass of liquid dispensed each time is accurately measured by controlling the opening of the butterfly valve and the gate valve, as well as by the automatic weighing device of the sedimentation reactor 5. The butterfly valve is a self-feedback regulating valve that automatically adjusts its opening based on the weight data fed back from the sedimentation reactor.
[0043] The equalization device quantitatively and evenly separates the precipitated slurry into 6 material cups; after the separation is completed, the centrifuge is turned on to complete the solid-liquid separation; the robotic arm 12 will grab the material cups one by one and pour the supernatant into the mother liquor storage tank 3, controlling the pouring speed and the pouring angle of 8 degrees to ensure that the solid material flows out together; after the solid-liquid separation is completed, the robotic arm 12 is remotely controlled to transfer the material cups one by one to the material cup rack of the calcining furnace; after the transfer is completed, the calcining furnace 8 is turned off, the vacuum pump is turned on, and the heating temperature range is set to heat the material.
[0044] The top of the sedimentation reactor 5 is sealed with a flange, and the flange has a through hole with a diameter larger than that of the inlet pipe. The bottom of the sedimentation reactor 5 is constructed by welding an elliptical head. The sedimentation reactor 5 is fixed by fixing it to the edge of the top flange, without making rigid connections to the inlet pipe, outlet, or other locations, thus avoiding stress concentration and breakage at the pipe connections.
[0045] The centrifuge is located at the bottom of the sedimentation reactor, with the centrifuge rack positioned 3 cm below the discharge pipe. The rack has six cup openings. Uniform discharge and automatic rack rotation and positioning are achieved through program control. The centrifugation speed and time can be automatically and remotely set. The centrifuge rack and cup openings are connected flexibly. Under centrifugal force, the cup openings gradually tilt inwards, causing the heavy components (solid precipitates) to settle at the bottom of the cups, achieving solid-liquid separation.
[0046] The calcining furnace 8 is equipped with a movement cylinder to raise and lower the furnace cover and insulation cover, and has remote control functionality. After the material transfer is completed, a furnace closing command is issued via the central control panel, which activates the furnace body lifting cylinder to slowly lower the furnace body. Once it reaches the designated position, the insulation layer automatically locks onto the material rack, and the locking device and vacuum system are activated, completing the furnace closing process. After calcination is completed, a furnace opening command is issued via the central control panel. The vacuum stops, and the air supply vents slowly release pressure. Once the pressure returns to atmospheric pressure, the insulation cover automatically rises, the locking device opens, and the furnace body slowly rises, completing the furnace opening process.
[0047] The robotic arm 12 is a five-axis robotic arm with high positioning precision and adjustable execution speed. It can smoothly complete actions such as pouring mother liquor, feeding precipitates, and discharging calcined materials.
[0048] The calcining furnace 8 is an electric resistance furnace, used in conjunction with the vacuum pump 10, and the calcining furnace 8 has a bell-shaped shape.
[0049] The integrated precipitation and calcination device is also equipped with a vacuum pump 10 and a hydraulic column 9. The vacuum pump 10 and the hydraulic column 9 are located at the lower part of the outer frame 2 of the device.
[0050] The outer edge of the integrated precipitation and calcination device is a sealing device 11, which encloses the entire equipment to prevent material from polluting the environment.
[0051] The precipitation and calcination method using the above-mentioned integrated precipitation and calcination apparatus includes the following steps:
[0052] 1) Preparation before precipitation: After the stock solution and precipitant are prepared, they are stored in precipitant tank 1. After the precipitation reaction vessel 5 is emptied, the sensor reading of the automatic weighing device is cleared to zero by the logic controller.
[0053] 2) Precipitation Feeding: The precipitate stock solution is quantitatively added to the precipitation reactor 5 through the feed pipe using an electromagnetic pump, and the stirrer is turned on. After the precipitate stock solution is added, the oxalic acid precipitant is quantitatively added to the precipitation reactor 5 through the precipitant feed pipe using an electromagnetic pump. After the precipitant is added, the precipitate solution is aged.
[0054] 3) Slurry equalization: After aging, the number of slurry to be evenly divided is set to 6 in the logic controller. Automatic dispensing is started. The control system performs logical calculations based on the measurement values of the weighing device. After completion, automatic feeding is started. The logic controller automatically controls the ball valve to open to an appropriate degree based on the feedback signal to complete the slurry dispensing.
[0055] 4) Repeat step 3 until all 6 cups of precipitated slurry have been dispensed;
[0056] 5) Centrifugation: The precipitated material settles to the bottom of the cup under the action of centrifugal force;
[0057] 6) Calcination: After solid-liquid separation, the robotic arm places the gripping cup on the calcining furnace cup rack to begin calcination.
[0058] Example 1
[0059] 1. Preparation before precipitation. After preparing the stock solution and precipitant, store them in precipitant tank 1. Turn on the automatic dispensing system, and after confirming that the precipitation reaction vessel 5 is emptied, reset the weighing sensor reading to zero through the logic controller.
[0060] 2. Precipitation Feeding. First, the calcium nitrate precipitation solution is metered and added to precipitation reactor 5 through the precipitation solution feed pipe using an electromagnetic pump. The agitator in precipitation reactor 5 is then turned on. After the precipitation solution is added, the logic controller displays a material weight of 302g. Next, oxalic acid precipitant is metered and added to precipitation reactor 5 through the precipitant feed pipe using an electromagnetic pump. The addition rate of the precipitant is controlled. After the precipitant is added, the logic controller displays a total material weight of 3310g. After the precipitant addition is complete, the precipitate solution is aged for 6 minutes.
[0061] 3. Slurry Distribution. After the aging period, the quantity to be evenly divided is set to 6 portions in the logic controller. Automatic dispensing is then initiated. The control system performs logical calculations based on the measurements from the weighing device, determining that each portion should contain 551.67g of precipitated slurry. After the calculation is complete, automatic feeding is initiated. The logic controller automatically controls the ball valve to open to the appropriate degree based on the feedback signal, completing the slurry dispensing.
[0062] 4. Repeat step 3 until all 6 cups of precipitated slurry have been dispensed. Weigh each container using a balance and subtract the tare weight to obtain the net weight of each batch: Batch 1, 548g; Batch 2, 554g; Batch 3, 550g; Batch 4, 549g; Batch 5, 553g; Batch 6, 5556g. The weight of the dispensed precipitated slurry is generally uniform, indicating a good overall result.
[0063] 5. After dispensing, set the centrifugation time to 5 minutes and the centrifugation speed to 500 rpm. The precipitated material settles to the bottom of the container under centrifugal force. The supernatant is then poured out by the robotic arm, showing that the centrifuged material has a low water content.
[0064] 6. After solid-liquid separation, the robotic arm places the gripper cup onto the calcining furnace's cup rack. Three calcination temperatures are set (first stage 80℃, hold for 10 min; second stage 120℃, hold for 5 min; third stage 350℃, hold for 30 min).
[0065] 7. After the reaction ends, manually calculate the system retention and throughput. It can be seen that the system retention is extremely small and is set as the inherent system retention. The throughput is >80g / h.
[0066] Therefore, it can be considered that the precipitation and calcination device can achieve high-efficiency precipitation and calcination processing capabilities.
[0067] The integrated precipitation and calcination apparatus and method of this invention features high processing efficiency, low retention, high equipment integration, high sensitivity, and high degree of automation, making it worthy of widespread application. It will provide technical support for the automation improvement of chemical solution precipitation and calcination processes.
Claims
1. A precipitation-calcination integrated apparatus, characterized by: The device comprises an electromagnetic pump, a liquid inlet pipe, a precipitant tank (1), an external device frame (2), a mother liquor tank (3), a centrifuge (4), a precipitation reactor (5), a high-level tank (6), a calcining furnace (8) and a mechanical arm (12). The precipitant tank (1) is located at the lower part of the external device frame (2), the centrifuge (4), the precipitation reactor (5), the high-level tank (6), the calcining furnace (8) and the mechanical arm (12) are located at the upper part of the external device frame (2). The liquid inlet pipe penetrates the precipitation reactor (5) and the high-level tank (6). The electromagnetic pump transports the precipitant stock solution and the precipitant from the precipitant tank (1) to the high-level tank (6) through the liquid inlet pipe, then enters the precipitation reactor (5), and then enters the mother liquor tank (3) located inside the centrifuge (4) through the discharge port of the precipitation reactor (5). The mechanical arm (12) transports the material between the calcining furnace (8) and the centrifuge (4). An annular centrifuge frame is arranged below the discharge port of the precipitation reactor (5), and six material cups are arranged on the annular centrifuge frame. The precipitation and calcination integrated device is also provided with a remote operation function. The operator sends an action instruction through the intermediate control console, and the mechanical arm (12) starts to execute the predetermined action after receiving the signal. Through remote control and program writing, each material cup is automatically rotated and positioned at the lower end of the discharge port. The rotating actuator is located inside the centrifuge (4) and drives the rotation of the annular centrifuge frame. The material cup is placed on the annular material frame. The lower end of the discharge port of the precipitation reactor (5) is provided with a valve group, which comprises a first valve and a second valve, which are pneumatic valves and electromagnetic valves respectively, and is used for completing the dropping of the precipitation slurry. The valve group is a uniform distribution device. The first valve is a gate valve, and the second valve is a butterfly valve. The opening of the butterfly valve and the gate valve and the automatic weighing device of the precipitation reactor (5) are controlled to accurately measure the mass of the liquid in each batch. The butterfly valve is a self-feedback regulating valve, which automatically adjusts the opening of the valve according to the weight data fed back by the precipitation reactor. The uniform distribution device uniformly separates the precipitation slurry in the six material cups. The calcining furnace (8) comprises a bottom disc and a bell-shaped cover. The bottom disc is provided with a material cup rack, which can accommodate six material cups at a time. An elevating heat preservation cover is arranged above the material cup rack. The heat preservation cover is buckled on the material rack after the cover of the calcining furnace (8) is closed. The mechanical arm (12) grasps the material cups one by one to pour the supernatant into the mother liquor tank (3), controls the pouring speed and the pouring angle of 8 degrees to ensure that the solid material flows out together. After the solid-liquid separation is completed, the mechanical arm (12) is remotely controlled to transport the material cups to the material cup rack of the calcining furnace (8) one by one.
2. The integrated precipitation-calcination apparatus of claim 1, wherein: The precipitation reactor (5) is provided with an automatic weighing device. After cleaning after one reaction, the automatic weighing device is automatically reset to zero through a logical algorithm.
3. The integrated precipitation-calcination apparatus of claim 2, wherein: The top of the precipitation reactor (5) is flange sealed, and a through hole with a larger aperture than the liquid inlet pipe is formed in the flange. The bottom of the precipitation reactor (5) is composed of an elliptical head welded together. The precipitation reactor (5) is fixed by the top flange edge.
4. The integrated precipitation-calcination apparatus of claim 3, wherein: The centrifuge is arranged at the lower end of the precipitation reactor (5). The centrifuge rack is located 3 cm below the discharge pipe. The centrifugal speed and time are automatically set remotely during the centrifugation process.
5. The integrated precipitation-calcination apparatus of claim 4, wherein: The calcining furnace (8) is provided with a moving cylinder to complete the lifting of the calcining furnace cover and the heat preservation cover, and has a remote control function; after the material is transferred, the central control panel issues a closing furnace command, the calcining furnace body lifting cylinder moves, the calcining furnace body slowly descends, the vacuum system starts, and the closing furnace action is completed; after the calcination is completed, the central control panel issues an opening furnace command, the vacuum stops, the heat preservation cover automatically rises, and the opening furnace is completed.
6. The integrated precipitation-calcination apparatus of claim 5, wherein: The mechanical hand (12) is a five-axis mechanical hand.
7. The integrated precipitation-calcination apparatus of claim 6, wherein: The precipitation and calcination integrated device is also provided with a vacuum pump (10), a hydraulic column (9) and a surrounding device (11); the vacuum pump (10) and the hydraulic column (9) are located at the lower part of the device outer frame (2); and the outer edge is the surrounding device (11).
8. The integrated precipitation-calcination apparatus of claim 7, wherein: The calcining furnace (8) is a resistance furnace, which is used together with the vacuum pump (10); and the shape of the calcining furnace (8) is a bell jar type.
9. A precipitation-calcination method using the precipitation-calcination integrated apparatus according to claim 8, characterized by: The method comprises the following steps: 1) preparation before precipitation: after the preparation of the precipitation stock solution and the precipitant is completed, the precipitation stock solution and the precipitant are stored in the precipitant tank (1); after the precipitation reactor (5) is emptied, the sensor of the automatic weighing device is reset to zero through the logic controller; 2) precipitation feeding: the precipitation stock solution is quantitatively added into the precipitation reactor (5) through the feeding pipe by the electromagnetic pump, and the stirrer is started; after the addition of the precipitation stock solution is completed, the oxalic acid precipitant is quantitatively added into the precipitation reactor (5) through the feeding pipe by the electromagnetic pump, and the precipitation solution is aged after the addition of the precipitant is completed; 3) slurry division: after aging, the number of 6 portions to be divided is set in the logic controller, the automatic packaging is started, the control system performs logical calculation according to the measurement value of the weighing device, after completion, the automatic unloading is started, the logic controller automatically controls the ball valve to open to an appropriate opening degree according to the feedback signal, and the slurry packaging is completed; 4) repeat step 3) until the six cups of precipitation slurry are packaged; 5) centrifugation: the precipitated material is settled at the bottom of the cup under the action of centrifugal force; 6) calcination: after the solid-liquid separation, the mechanical arm places the cup in the calcining furnace cup rack, and the calcination starts.
10. The precipitation calcination process according to claim 9, characterized in that: In step 1), the precipitation stock solution is calcium nitrate, the aging time in step 2) is 6 minutes, the centrifugation time in step 3) is 5 minutes, and the centrifugation speed is 500 rpm.
Citation Information
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