A processing device and method for extracting iron phosphate using phosphating slag
By designing a treatment device including solid-liquid separator, phosphating slag pretreatment device, solid-liquid separation and cleaning device, high-pressure hydrothermal reactor, etc., the problems of low utilization rate of phosphating slag and environmental pollution are solved, and high-quality Extraction of purity iron phosphate and sustainable use of the environment.
Patent Information
- Application Number
- CN202310577171.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-22
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2043-05-22
AI Technical Summary
In the prior art, the utilization rate of phosphated slag is low and the environmental pollution is severe. In the prior art, the prior art fails to effectively remove impurities when treating phosphated slag, resulting in low purity of extracted iron phosphate.
A treatment device including a solid-liquid separator, a phosphating slag pretreatment device, a solid-liquid separation and cleaning device, a high-pressure hydrothermal reactor, an acid storage tank, a dryer and a material storage tank are designed. The device removes impurities in the phosphating slag and extracts high-purity iron phosphate through solid-liquid separation, pretreatment, hydrothermal reaction and other steps.
The utilization rate of phosphating slag is significantly improved, environmental pollution is reduced, and the purity of iron phosphate is improved through pretreatment and hydrothermal reaction.
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Figure CN116514085B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to a processing device and a method for extracting iron phosphate by utilizing phosphating slag, and belongs to the technical field of phosphating slag processing. Background Art
[0002] Phosphating technology is now widely used in the automotive industry and has become one of the most commonly used metal surface treatment technologies in this field. Phosphating slag is a white waste slag produced during the phosphating process. As the reaction continues, the amount of phosphating slag is also increasing sharply. If a large amount of phosphating slag is accumulated in the phosphating tank and is not treated in time, it will not only affect the quality of the phosphating film and shorten the service life of the phosphating solution, but also damage the phosphating equipment. Since the main components of phosphating slag are iron phosphate, zinc phosphate, and other metal ions such as calcium, copper, and nickel, if it is directly discharged into the soil without any treatment or simply landfilled, it will cause certain environmental pollution and waste of resources. Therefore, it is of great significance to study the resource utilization of phosphating slag.
[0003] The Chinese utility model patent with the authorization announcement number CN210874249U discloses a multi-stage precipitation separation system for solid-liquid separation of phosphating slag. This invention only separates the phosphating slag from the phosphating liquid to improve the solid-liquid separation efficiency of the phosphating slag. The phosphating slag is not further harmlessly treated and still has a certain impact on the environment. Therefore, it is necessary to further study, improve and improve the technology and methods for the rational use of phosphating slag.
[0004] The Chinese utility model patent with the authorization announcement number CN210795775U discloses a phosphating slag recycling treatment mechanism, including a reactor, a water tower, a solid-liquid separator, a flash drying tower, a filtrate secondary treatment system, and several connecting pipes. A water tower is provided on one side of the reactor, and the horizontal height of the water tower is higher than the horizontal height of the reactor. The water outlet end of the water tower is connected with the water inlet end of the reactor through a connecting pipe. A solid-liquid separator is provided on the other side of the reactor. The discharge port end of the reactor is connected with the feed port end of the solid-liquid separator through a connecting pipe. The sides of the solid-liquid separator are respectively provided with a solid discharge port of the solid-liquid separator and a liquid discharge port of the solid-liquid separator. The solid discharge port of the solid-liquid separator is connected to the upper feed port end of the flash drying tower through a connecting pipe, and the liquid discharge port of the solid-liquid separator is connected to the filtrate secondary treatment system. This patent can add water to the phosphating slag and heat it to produce hydroxy ferric phosphate, which improves the utilization rate of the phosphating slag to a certain extent and reduces the pollution to the environment. However, this patent directly introduces the phosphating slag into the reactor without pretreatment, and the impurities in the phosphating slag cannot be removed. The impurities are in the hydroxy ferric phosphate finally produced, which reduces the purity of the hydroxy ferric phosphate. The filtrate secondary treatment system of the above patent is composed of three independent sedimentation tanks and a collection tank connected together. The overall space occupied is large, and the material transportation distance is long, and the overall filtration efficiency is low. Summary of the invention
[0005] One of the purposes of the present invention is to provide a processing device for extracting iron phosphate using phosphating slag, so as to solve the technical defects of low utilization rate of phosphating slag produced by the phosphating process in the prior art and environmental pollution.
[0006] In order to solve the above problems, the technical scheme adopted by the present invention is: a processing device for extracting iron phosphate from phosphating slag, comprising a solid-liquid separator, a phosphating slag pretreatment device, a solid-liquid separation cleaning device, a high-pressure hydrothermal reactor, an acid storage tank, a dryer and a storage tank; the solid-liquid separator is used to separate the phosphating liquid and the phosphating slag generated in the phosphating process; the phosphating slag pretreatment device is connected to the solid-liquid separator, phosphoric acid is added to the phosphating slag separated by the solid-liquid separator in the phosphating slag pretreatment device, and heating and stirring are carried out in the phosphating slag pretreatment device to obtain a solid-liquid mixed product of the phosphating slag and phosphoric acid; the solid-liquid separation cleaning device is connected to the phosphating slag pretreatment device, and is used to separate the solid of the phosphating slag and phosphoric acid reacted in the phosphating slag pretreatment device. The high-pressure hydrothermal reactor is connected to the solid-liquid separation and cleaning device, and is used to perform a hydrothermal reaction on the solid product after being cleaned and separated by the solid-liquid separation and cleaning device after adding phosphoric acid, and the solid product after the hydrothermal reaction is transported to the solid-liquid separation and cleaning device for cleaning and separation to obtain iron phosphate; the acid storage tank is used to hold phosphoric acid, and the phosphating slag pretreatment device and the high-pressure hydrothermal reactor are both connected to the acid storage tank, and the acid storage tank is used to provide phosphoric acid to the phosphating slag pretreatment device and the high-pressure hydrothermal reactor when in use; the dryer is connected to the solid-liquid separation and cleaning device, and is used to dry the iron phosphate after being cleaned by the solid-liquid separation and cleaning device, and the storage tank is connected to the dryer, and is used to store the dried iron phosphate. The present invention extracts iron phosphate from the phosphating slag generated in the phosphating process, and the phosphating liquid after filtering the phosphating slag can be continuously used in the phosphating process, which greatly improves the utilization rate of the phosphating slag compared with direct discharge. On the other hand, compared with the prior art of directly discharging or landfilling the phosphating slag, the present invention reduces the pollution to the environment. Before the phosphating slag enters the reactor for reaction, the present invention first performs pretreatment in the phosphating slag pretreatment device to remove impurities therein, and after the reaction, the solid-liquid separation and cleaning device separates and cleans the solid-liquid reactants, which can improve the purity of the iron phosphate extracted from the phosphating slag.
[0007] As a further improvement of the present invention, the phosphating slag pretreatment device is connected to the high-pressure hydrothermal reactor by a fifth pipeline, a seventh valve and an eighth valve are arranged on the fifth pipeline, the fifth pipeline is connected to the acid storage tank by a sixth pipeline, and the connection between the sixth pipeline and the fifth pipeline is located between the seventh valve and the eighth valve. The present invention connects the acid storage tank, the phosphating slag pretreatment device and the high-pressure hydrothermal reactor through the fifth pipeline and the sixth pipeline, and phosphoric acid can be added to the phosphating slag pretreatment device and the high-pressure hydrothermal reactor simultaneously or separately by opening and closing the seventh valve and the eighth valve.
[0008] As a further improvement of the present invention, a water tower is further included, which is connected to the solid-liquid separation cleaning device and is used to add cleaning water into the solid-liquid separation cleaning device. The present invention is provided with a water tower, and when in use, the water tower can provide cleaning water to the solid-liquid separation cleaning device, which is used to clean the solids in the solid-liquid separation cleaning device and separate the solid-liquid mixture.
[0009] As a further improvement of the present invention, the phosphating slag pretreatment device is connected to the solid-liquid separation cleaning device by a first pipeline, and a second valve and a third valve are arranged on the first pipeline, the solid-liquid separation cleaning device is connected to the high-pressure hydrothermal reactor by a third pipeline, and a fourth valve and a fifth valve are arranged on the third pipeline, the high-pressure hydrothermal reactor is connected to the first pipeline by a second pipeline, and the second pipeline and the first pipeline are connected at a position between the second valve and the third valve, the dryer is connected to the third pipeline by a fourth pipeline, and the fourth pipeline and the third pipeline are connected at a position between the fourth valve and the fifth valve, and a sixth valve is arranged on the fourth pipeline. When the fourth valve and the fifth valve are opened and the sixth valve is closed, the present invention can connect the solid-liquid separation cleaning device with the high-pressure hydrothermal reactor, so that the phosphating slag separated and cleaned in the solid-liquid separation cleaning device is transported to the high-pressure hydrothermal reactor, and when the fifth valve is closed and the fourth valve and the sixth valve are opened, the solid-liquid separation cleaning device can be connected to the dryer to collect the extracted iron phosphate, so that the solid-liquid separation cleaning device in the present invention can use the same outlet to simultaneously connect the high-pressure hydrothermal reactor and the dryer, reducing the number of openings on the solid-liquid separation cleaning device.
[0010] As a further improvement of the present invention, it also includes a liquid storage tank, which is connected to the solid-liquid separation cleaning device and is used to store the liquid after the solid-liquid separation cleaning device cleans. The present invention is provided with a liquid storage tank for collecting the cleaning water after the solid-liquid separation cleaning device cleans the phosphating slag or ferric phosphate.
[0011] As a further improvement of the present invention, the solid-liquid separation and cleaning device includes a base, a box body is arranged on the upper part of the base, the box body is divided into a separation chamber and a cleaning chamber by a partition, a feed port is provided at the top of one end of the separation chamber, the separation chamber is communicated with the end of the cleaning chamber away from the feed port, a spiral conveying device is provided in the separation chamber, which is used to push the solid matter in the separation chamber toward the side away from the feed port and drop it into the cleaning chamber, a drain port is provided at the bottom of the separation chamber on the side close to the feed port, which is used to discharge the liquid matter in the separation chamber; a water inlet is provided on the upper part of the cleaning chamber near one end of the feed port, which is used to add water to the cleaning chamber, and a stirring shaft for fixing a plurality of first stirring paddles is provided in the cleaning chamber, which is used to stir the water and Solid matter; a rotating drum is rotatably arranged at the lower part of the base, and a solid phase outlet and a liquid phase outlet are respectively arranged at two ends of the rotating drum, and a first conveying shaft with a first spiral blade fixed thereon is rotatably arranged in the rotating drum, and the first conveying shaft is a hollow structure, and one end of the first conveying shaft is connected to the bottom of one end of the cleaning chamber by a rotating joint and a seventh pipeline, and a material dividing port is radially arranged on the first conveying shaft, and the solid-liquid mixture in the cleaning chamber is conveyed to the first conveying shaft through the seventh pipeline, and discharged into the rotating drum through the material dividing port, wherein the liquid objects flow to the liquid phase outlet and are discharged from the rotating drum, and the solid objects are pushed to the solid phase outlet by the first spiral blade and are discharged from the rotating drum, and a differential is arranged on the first conveying shaft for adjusting the rotation speed of the first conveying shaft to be less than the rotation speed of the rotating drum. The separation chamber in the solid-liquid separation and cleaning device of the present invention performs preliminary separation of solid and liquid, the separated liquid is discharged from the separation chamber, the solid enters the cleaning chamber, and is cleaned in the cleaning chamber, and finally centrifugal separation is performed in the rotating drum, which shortens the time of solid-liquid separation and improves the efficiency of solid-liquid separation. The solid-liquid separation and cleaning device of the present invention occupies a smaller space as a whole, and the material is transported over a short distance in the present invention, which improves the efficiency of solid-liquid separation and cleaning. The rotation speed of the first conveying shaft and the first spiral blade in the present invention is less than the rotation speed of the rotating drum, and the rotating drum rotates at a high speed to achieve a centrifugal effect.
[0012] As a further improvement of the present invention, a first motor is installed at one end of the seventh pipeline on the base, and the first motor is connected to the drum by a transmission belt. An electrical control system is arranged at the other end of the base, and one end of the stirring shaft and the spiral conveying device are both connected to the electrical control system and driven to rotate by a second motor in the electrical control system. The present invention connects the separation chamber and the drum through the seventh pipeline, and can convey the solid-liquid mixture in the separation chamber to the drum. The solid-liquid separation and cleaning device in the present invention only needs two motors, and the overall structure is simpler.
[0013] Another object of the present invention is to provide a method for extracting iron phosphate using phosphating slag, which is used to extract iron phosphate from phosphating slag. The technical solution adopted by the present invention is: a method for extracting iron phosphate using phosphating slag, comprising the following steps:
[0014] Step 1: using a solid-liquid separator to separate the phosphating liquid and phosphating slag produced during the phosphating process.
[0015] Step 2: adding phosphoric acid to the phosphating slag separated in step 1 in a phosphating slag pretreatment device, and stirring at 60 to 80° C. for 4 to 6 hours to obtain a solid-liquid mixture.
[0016] Step 3, performing solid-liquid separation on the mixed liquid mixture of step 2 in a solid-liquid separation and cleaning device, and cleaning the solid objects therein with water.
[0017] Step 4, subjecting the solid object cleaned in step 3 to a hydrothermal reaction in a high-pressure hydrothermal reactor to obtain iron phosphate.
[0018] Step 5, washing the iron phosphate obtained in step 4 in a solid-liquid separation and washing device.
[0019] Step 6, collecting iron phosphate.
[0020] The invention extracts iron phosphate from phosphating slag to improve the utilization rate of the phosphating slag and reduce the pollution to the environment.
[0021] As a further improvement of the present invention, the reaction temperature in the high-pressure hydrothermal reactor in step 4 is 180-220° C., the pressure is 1.2-1.5 MPa, and the reaction time is 4-6 hours. The iron phosphate obtained under the reaction conditions has high purity, and the large iron phosphate particles in the phosphating slag are modified under high temperature and high pressure, thereby improving the shape of the iron phosphate particles.
[0022] As a further improvement of the present invention, step 6 comprises:
[0023] Step 6.1, using a dryer to dry the iron phosphate.
[0024] Step 6.2, collecting the dried iron phosphate into a storage tank.
[0025] The present invention first dries the ferric phosphate and then stores it, which is more conducive to the preservation of the ferric phosphate.
[0026] In summary, the beneficial effects of the present invention are as follows: the present invention purifies solid waste phosphating slag into iron phosphate, which greatly improves the utilization rate of the phosphating slag and reduces environmental pollution; the solid-liquid separation and cleaning device in the present invention can clean the solid while separating the solid and the liquid to ensure the purity of the product, and the device is divided into two parts: preliminary separation and centrifugal separation, which shortens the separation time and greatly improves the separation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 It is a structural schematic diagram of the present invention.
[0028] Figure 2 It is a structural schematic diagram of the solid-liquid separation and cleaning device in the present invention.
[0029] Among them: 1. Phosphating tank; 2. Solid-liquid separator; 3. Phosphating slag pretreatment device; 4. Solid-liquid separation and cleaning device; 5. High-pressure hydrothermal reactor; 6. Dryer; 7. Acid storage tank; 8. Liquid storage tank; 9. Water tower; 10. Storage tank; V1. First valve; V2. Second valve; V3. Third valve; V4. Fourth valve; V5. Fifth valve; V6. Sixth valve; V7. Seventh valve; V8. Eighth valve; V9. Ninth valve; V10. Tenth valve; 401. Base; 402. Shock absorber; 403. Electrical control system; 404. Differential; 405. Drive shaft; 406. Box; 407. Cover; 408. Spiral blade; 409. Agitator; 410. Feed hopper; 411. Partition; 412. Water inlet; 413. Discharge port; 414. Feed port; 415. Bearing sleeve; 416. Drive shaft; 417. First motor; 418. Drum; 419. Spiral; 420. Distributor port; 421. Solid phase outlet; 422. Liquid phase outlet. DETAILED DESCRIPTION
[0030] The specific implementation of the present invention is further described below in conjunction with the accompanying drawings. Example 1
[0031] like Figure 1 The processing device for extracting iron phosphate using phosphating slag shown includes a solid-liquid separator 2, a phosphating slag pretreatment device 3, a solid-liquid separation and cleaning device 4, a high-pressure hydrothermal reactor 5, an acid storage tank 7, a dryer 6 and a storage tank 10.
[0032] The solid-liquid separator 2 in the present invention is used to separate the phosphating liquid and the phosphating slag produced in the phosphating process. The structure of the solid-liquid separator 2 is the prior art. The solid-liquid separator 2 is preferably connected to the phosphating tank 1 by a ninth pipeline, and a first valve V1 is installed on the ninth pipeline. When the first valve V1 is opened, the phosphating liquid and the phosphating slag produced after the phosphating treatment of the workpiece in the phosphating tank 1 can be directly transported to the solid-liquid separator 2 through the ninth pipeline and separated in the solid-liquid separator 2. The present invention is provided with a tenth pipeline, and the two ends of the tenth pipeline are respectively extended into the solid-liquid separator 2 and the phosphating tank 1, and a water pump is arranged on the tenth pipeline. The phosphating liquid separated by the solid-liquid separator 2 can be transported back to the phosphating tank 1 through the tenth pipeline for reuse.
[0033] The phosphating slag pretreatment device 3 of the present invention is connected to the solid-liquid separator 2 by an eighth pipeline. The shell 301 of the phosphating slag pretreatment device 3 is provided with an agitator 302, and the agitator 302 includes a rotating shaft, a stirring motor and a plurality of second stirring paddles. The rotating shaft is arranged in a vertical direction, and the stirring motor is installed on the top of the shell 301. The output shaft of the stirring motor is arranged vertically downward and connected to the top of the rotating shaft. The second stirring paddle is fixed on the rotating shaft in a radial direction. The stirring motor drives the rotating shaft to rotate, and the second stirring paddle on the rotating shaft stirs the material in the phosphating slag pretreatment device 3. Stirring and mixing, a heating device 303 and a controller 304 are provided at the bottom of the shell 301 of the phosphating slag pretreatment device 3, and the control device 304 controls the heating of the material in the shell 301. The heating device 303 and the controller 304 in the present invention are both prior art, and the present invention will not describe them in detail. When in use, the phosphating slag separated by the solid-liquid separator 2 is transported to the phosphating slag pretreatment device 3 through the eighth pipeline, phosphoric acid is added to the phosphating slag pretreatment device, and heating and stirring reaction are carried out in the phosphating slag pretreatment device 3 to obtain a solid-liquid mixed product of the phosphating slag and phosphoric acid. The phosphating slag pretreatment device 3 in the present invention pretreats the phosphating slag to preliminarily remove impurities in the phosphating slag.
[0034] The solid-liquid separation and cleaning device 4 is connected to the phosphating slag pretreatment device 3, and is used to separate and clean the solid-liquid mixed product of the phosphating slag and phosphoric acid reacted in the phosphating slag pretreatment device 3. The phosphating slag pretreatment device 3 in the present invention is connected to the solid-liquid separation and cleaning device 4 by a first pipeline, and a second valve V2 and a third valve V3 are provided on the first pipeline, wherein the second valve V2 is located on a side close to the phosphating slag pretreatment device 3, and the third valve V3 is located close to a side of the solid-liquid separation and cleaning device 4.
[0035] The high-pressure hydrothermal reactor 5 in the present invention is connected to the solid-liquid separation and cleaning device 4, and is used to perform a hydrothermal reaction on the solid product cleaned and separated by the solid-liquid separation and cleaning device 4 after adding phosphoric acid, and transport the solid product after the hydrothermal reaction to the solid-liquid separation and cleaning device 4 for cleaning and separation to obtain iron phosphate. The solid-liquid separation and cleaning device 4 is connected to the high-pressure hydrothermal reactor 5 by a third pipeline, and a fourth valve V4 and a fifth valve V5 are arranged on the third pipeline, wherein the fourth valve V4 is located on a side close to the solid-liquid separation and cleaning device 4, and the fifth valve V5 is located on a side close to the high-pressure hydrothermal reactor 5.
[0036] The high-pressure hydrothermal reactor 5 in the present invention is connected to the first pipeline by a second pipeline, and the connecting portion between the second pipeline and the first pipeline is located between the second valve V2 and the third valve V3. An eleventh valve V11 is arranged on the second pipeline, so that when the eleventh valve V11 is closed and the second valve V2 and the third valve V3 are opened, the phosphating slag pretreatment device 3 and the solid-liquid separation cleaning device 4 can be connected, and when the second valve V2 is closed and the eleventh valve V11 and the third valve V3 are opened, the solid-liquid separation cleaning device 4 and the high-pressure hydrothermal reactor 5 can be connected. When the third valve V3 is closed, the solid-liquid separation cleaning device 4 is not connected to the high-pressure hydrothermal reactor 5 and the phosphating slag pretreatment device 3. The dryer 6 in the present invention is connected to the solid-liquid separation cleaning device 4, and is used to dry the iron phosphate after cleaning by the solid-liquid separation cleaning device 4. The storage tank 10 is connected to the drying device. The dryer 6 is connected to the third pipeline and is used to store the dried iron phosphate. The dryer 6 in the present invention is connected to the third pipeline by a fourth pipeline. The connection point between the fourth pipeline and the third pipeline is located between the fourth valve V4 and the fifth valve V5. The fourth pipeline is provided with a sixth valve V6. When the sixth valve V6 is closed and the fourth valve V4 and the fifth valve V5 are opened at the same time, the solid-liquid separation cleaning device 4 is connected to the high-pressure hydrothermal reactor 5. When the fifth valve V5 is closed and the fourth valve V4 and the sixth valve V6 are opened at the same time, the solid-liquid separation cleaning device 4 is connected to the dryer 6. When the fourth valve V4 is closed, the solid-liquid separation cleaning device 4 is not connected to the high-pressure hydrothermal reactor 5 and the dryer 6. When the dryer 6 is connected to the solid-liquid separation cleaning device 4, the iron phosphate cleaned by the solid-liquid separation cleaning device 4 enters the dryer 6, and after the iron phosphate is dried, it enters the storage tank for collection and storage.
[0037] The acid storage tank 7 in the present invention is used to hold phosphoric acid. The phosphating slag pretreatment device 3 and the high-pressure hydrothermal reactor 5 are both connected to the acid storage tank 7. The acid storage tank 7 is used to provide phosphoric acid to the phosphating slag pretreatment device 3 and the high-pressure hydrothermal reactor 5 when in use. The phosphating slag pretreatment device 3 in the present invention is connected to the high-pressure hydrothermal reactor 5 by a fifth pipeline. A seventh valve V7 and an eighth valve V8 are provided on the fifth pipeline. The seventh valve V7 is located on a side close to the phosphating slag pretreatment device 3, and the eighth valve V8 is located on a side close to the high-pressure hydrothermal reactor. On one side of the kettle 5, the fifth pipeline is connected to the acid storage tank 7 by the sixth pipeline, and the connection between the sixth pipeline and the fifth pipeline is located between the seventh valve V7 and the eighth valve V8. When the seventh valve V7 is opened, the acid storage tank 7 is connected to the phosphating slag pretreatment device 3, and the acid storage tank 7 can add phosphoric acid to the phosphating slag pretreatment device 3 through the sixth pipeline and the fifth pipeline. When the eighth valve V8 is opened, the acid storage tank 7 is connected to the high-pressure hydrothermal reactor 5, and the acid storage tank 7 can add phosphoric acid to the high-pressure hydrothermal reactor 5 through the sixth pipeline and the fifth pipeline.
[0038] In order to facilitate adding water to the solid-liquid separation cleaning device 4 to clean the phosphating slag or iron phosphate, the present invention is provided with a water tower 9 for holding cleaning water, the water tower 9 is connected to the solid-liquid separation cleaning device 4 by an eleventh pipeline, and a ninth valve V9 is provided on the eleventh pipeline. When the ninth valve V9 is opened, the cleaning water for cleaning the phosphating slag or iron phosphate can be added from the water tower to the solid-liquid separation cleaning device 4. In order to collect the clear liquid water after the solid-liquid separation cleaning device is cleaned, the present invention is provided with a liquid storage tank 8, the liquid storage tank 8 is connected to the solid-liquid separation cleaning device 4, and is used to store the liquid after the solid-liquid separation cleaning device 4 is cleaned.
[0039] like Figure 2 As shown, the solid-liquid separation cleaning device 4 in the present invention includes a base 401, a plurality of shock absorbers 402 are arranged at the bottom of the base 401 to reduce the vibration of the solid-liquid separation cleaning device 4 when in use, a box body 406 is arranged on the upper part of the base 401, and the box body 406 is divided into a separation chamber and a cleaning chamber by a partition 411, and the partition 411 is welded and fixed to the inner wall of the box body 406, wherein the separation chamber is located above the cleaning chamber, and a feed port 410 is opened at the top of one end of the separation chamber, as shown in FIG. Figure 2 As shown, a feed port 410 is opened at the top of the right end of the separation chamber, and the feed port 410 is connected to the first pipe. The best embodiment of the present invention is to provide a feed funnel at the feed port 410, and the end of the first pipe extends into the feed funnel to facilitate the material in the first pipe to enter the separation chamber of the solid-liquid separation and cleaning device 4. The separation chamber and the cleaning chamber are connected at the end away from the feed port 410, that is, the left end of the separation chamber is connected to the left end of the cleaning chamber. The present invention provides a through hole running through the upper and lower parts of the partition 411 at the left end thereof for connecting the separation chamber and the cleaning chamber. The present invention is provided with a spiral conveying device in the separation chamber for pushing the solid matter in the separation chamber toward the side away from the feed port 410 and dropping it into the cleaning chamber. The spiral conveying device includes a second spiral blade 408 and a second conveying shaft, and the two ends of the second conveying shaft are respectively rotatably connected to the left and right ends of the box body 406 by bearings. The left end of the second conveying shaft extends out of the box body 406 and is connected to a driving device for driving its rotation. The second spiral blade 408 is fixed on the second conveying shaft, wherein the pitch of the second spiral blade 408 located at one end (i.e., the left end) of the feed port 410 is greater than the pitch of the end where the separation chamber and the cleaning chamber are connected, and a drain port is opened on the side of the bottom of the separation chamber close to the feed port 410 for discharging liquid substances in the separation chamber. The present invention preferably sets the bottom of the separation chamber as an inclined surface, and the end where the drain port is located is slightly inclined downward to facilitate the discharge of liquid in the separation chamber.
[0040] The present invention has a water inlet 412 on the upper part of the cleaning chamber located near one end of the feed port 410 for adding cleaning water into the cleaning chamber. A stirring shaft with multiple first stirring paddles 409 fixed thereon is provided in the cleaning chamber for stirring the water and solid matter in the cleaning chamber. The stirring shaft is rotatably connected to the box 406. The solid objects entering the cleaning chamber from the separation chamber are mixed with the cleaning water, and the first stirring paddle 409 is driven by the stirring shaft to rotate for stirring and cleaning. Both ends of the stirring shaft in the present invention are also rotatably connected to the box 406 by bearings. The left end of the stirring shaft extends out of the box 406 and is connected to a driving device for driving it to rotate. The present invention optimally uses the same driving device to drive the stirring shaft and the second conveying shaft to rotate.
[0041] The present invention is provided with a rotating drum 418 at the lower part of the base 401, wherein the rotating drum 418 is rotatably connected to the bearing seat 415 on the base 401, and the left and right ends of the rotating drum 418 are respectively provided with a solid phase outlet 421 and a liquid phase outlet 422, wherein the inner diameter of the end of the rotating drum 418 provided with the solid phase outlet 421 is smaller than the inner diameter of the end of the rotating drum 418 provided with the liquid phase outlet 422, and a first conveying shaft with a first spiral blade fixed thereto is rotatably provided in the rotating drum 418, the first conveying shaft is a hollow structure and is coaxially provided with the rotating drum 418, both ends of the first conveying shaft extend out of the rotating drum 418, the first conveying shaft is rotatably connected to the rotating drum 418, and one end of the first conveying shaft is connected to the bottom of one end of the cleaning chamber by a rotating joint and a seventh pipeline. A material distribution port 420 is radially opened on the first conveying shaft to communicate with the hollow part of the first conveying shaft and the drum 418. The solid-liquid mixture in the cleaning chamber is transported to the first conveying shaft through the seventh pipeline, and discharged into the drum 418 from the material distribution port 420 on the first conveying shaft, wherein the liquid objects flow to the liquid phase outlet 422 and are discharged from the drum 418, and the solid objects are pushed to the solid phase outlet 421 by the first spiral blade and are discharged from the drum 418. A differential 404 is installed on the left end of the first conveying shaft in the present invention, which is used to adjust the rotation speed of the first conveying shaft to be less than the rotation speed of the drum 418, so that the drum 418 can rotate at a high speed. The differential 404 in the present invention is a prior art and will not be described in detail in the present invention.
[0042] The present invention is best to fix end plates at both ends of the drum 418, the first conveying shaft passes through the two end plates, and uses bearings to rotate relative to the end plates, a cover shell 407 is provided at the bottom of the base 401, the drum 418 is arranged in the cover shell 407, and a discharge cavity is provided at each end of the cover shell 407, and the discharge cavity is formed by splicing and separating plates, and the two ends of the drum 418 extend into the two discharge cavities respectively, and the solid phase outlet 421 and the liquid phase outlet 422 are respectively provided at the end plates at the two ends of the drum 418. The solid and liquid substances discharged from the solid phase outlet 421 and the liquid phase outlet 422 are discharged from the two discharge cavities respectively. The third pipeline in the present invention and the pipeline connected to the liquid storage tank are connected to the two discharge cavities respectively to avoid the interference of the rotation of the drum 418 on the discharge. In the present invention, connecting sleeves are fixed on the end plates at both ends of the drum 418, wherein the first output shaft passes through the connecting sleeve, and the connecting sleeve is rotatably connected with the base 401 and the bearing seat 415 thereon.
[0043] The present invention installs a first motor 417 at one end of the seventh pipeline on the base 401, and the output shaft of the first motor 417 is connected to the connecting sleeve on the end plate at one end of the drum 418 by a transmission belt 416. The present invention arranges an electrical control system 403 at the other end of the base 401. The electrical control system 403 is a prior art, and a gear transmission structure is arranged in the electrical control system 403, which will not be described in detail in the present invention. In the present invention, one end of the second conveying shaft of the stirring shaft and the screw conveying device are connected to the electrical control system 403, and are driven to rotate by the second motor in the electrical control system. The housing of the differential 404 in the present invention is connected to the connecting sleeve on the end plate at the left end of the drum 418, the output shaft of the differential 404 is connected to the first conveying shaft, and the input shaft of the reducer 404 is connected to the second motor (not shown in the figure) installed in the electrical control system 403. Therefore, in the present invention, only one second motor is required to be arranged in the electrical control system 403. The first motor 417 drives the drum 418 to rotate and also drives the housing of the reducer 404 to rotate. Since the input shaft of the reducer 404 is controlled by the second motor, the planetary gear in the differential 404 is driven according to the designed transmission relationship ( That is, the speed of the output shaft of the differential 404 is slightly slower than the speed of the differential housing), and the power of the output shaft of the differential 404 is transmitted to the first conveying shaft, thereby driving the spiral composed of the first conveying shaft and the first spiral blade and the drum 418 to rotate in the same direction but at different speeds. In the present invention, since the drum and the spiral rotate relative to each other, the first spiral blade takes effect, and the solid-liquid mixture in the drum 418 is discharged from the feed outlet 420 after centrifugation. The solid deposited on the inner wall of the drum 418 is scraped off by the first spiral blade and rolled to the fixed outlet 421, and the liquid is discharged from the liquid phase outlet 422. Example 2
[0044] This embodiment is a method for extracting iron phosphate using phosphating slag, using the processing device for extracting iron phosphate using phosphating slag in Example 1, and the method specifically includes the following steps:
[0045] Step 1, using a solid-liquid separator 2 to separate the phosphating liquid and the phosphating slag generated during the phosphating process, specifically, opening the first valve V1, so that the phosphating slag in the phosphating tank 1 is transported to the liquid separator 2 together with the phosphating liquid, so that the phosphating slag and the phosphating liquid are separated, and then closing the first valve V1, and the separated phosphating liquid is returned to the phosphating tank 1 through the tenth pipeline to continue to be used for phosphating the workpiece.
[0046] Step 2, close the second valve V2 and the seventh valve V7, transport the phosphating slag separated in step 1 to the phosphating slag pretreatment device 3 through the eighth pipeline, open the seventh valve V7, add phosphoric acid into the phosphating slag pretreatment device 3 and then close the seventh valve V7, control the heating device 303 by the controller 304, heat the temperature in the shell 301 to 60-80°C, start the first motor 417, drive the rotating shaft and the second stirring paddle to rotate, make the rotating shaft rotate at a speed of 1000-1200r / min (revolutions / minute), stir for 4-6h, and obtain a solid-liquid mixed product. In the present invention, the acid storage tank 7 contains a mixed solution of phosphoric acid and water with a mass ratio of 1: (3-5). The temperature, stirring speed and stirring time in the present invention can more fully remove impurities in the phosphating slag.
[0047] In step 3, the eleventh valve V11 and the fourth valve V4 are closed, and the second valve V2 and the third valve V3 are opened, so that the solid-liquid mixed product obtained by the reaction in step 2 is transported to the solid-liquid separation and cleaning device 4, and then the second valve V2 and the third valve V3 are closed, and the solid-liquid separation and cleaning device 4 performs solid-liquid separation on the mixed liquid mixture of step 2, and cleans the solid objects therein with water.
[0048] Step 3 specifically includes:
[0049] Step 3.1, the solid-liquid mixed product transported by the phosphating slag pretreatment device 3 through the first pipeline enters the separation chamber from the feed funnel at the feed port 410, the screw conveying device is turned on, and the second spiral blade 408 transports the solid phosphating slag in the direction away from the feed port 410, and falls downward from the through hole on the partition 411 into the cleaning chamber, and the liquid substance in the separation chamber is discharged from the drain port, and the liquid discharged from the drain port can be collected in a special container.
[0050] Step 3.2: Washing water is introduced into the washing chamber from the water inlet 412, the stirring shaft rotates, and the first stirring paddle 409 stirs and mixes the solid phosphating slag in the washing chamber in the washing water for washing.
[0051] Step 3.3, the solid-liquid mixture in the cleaning chamber is transported to the first conveying shaft via the seventh pipeline, and enters the drum 418 from the distribution port 420 on the first conveying shaft, wherein the cleaning water is discharged from the liquid phase outlet 422 into the liquid storage tank 8 for collection, and the solid phosphating slag is transported to the solid phase outlet 421 by the first spiral blade, and enters the third pipeline from the solid phase outlet 421.
[0052] Step 4, close the sixth valve V6 and the tenth valve V10 provided on the high-pressure hydrothermal reactor 5, open the fourth valve V4 and the fifth valve V5, transport the solid object (phosphating slag) cleaned in step 3 to the high-pressure hydrothermal reactor 5 through the third pipeline, then close the fifth valve V5, open the eighth valve V8, add phosphoric acid from the acid storage tank 7 to the high-pressure hydrothermal reactor 5, and then close the eighth valve V8, and perform a hydrothermal reaction in the high-pressure hydrothermal reactor 5. The reaction temperature in the high-pressure hydrothermal reactor 5 is 180-220° C., the pressure is 1.2-1.5 MPa, the reaction time is 4-6 hours, and iron phosphate is obtained after the reaction. The mass ratio of the mixed solution of phosphoric acid and water added to the high-pressure hydrothermal reactor 5 of the present invention to the phosphating slag is 1:1, so that the reaction is more complete.
[0053] Step 5, open the tenth valve V10, release the pressure in the high-pressure hydrothermal reactor 5, close the second valve V2, open the eleventh valve V11 and the third valve V3, and transport the iron phosphate obtained in step 4 to the solid-liquid separation and cleaning device 4 via the second pipeline and the third pipeline, and then close the third valve V3, and clean the iron phosphate obtained in step 4 in the solid-liquid separation and cleaning device 4. The cleaning method is the same as step 3. Please refer to step 3 for details, and the present invention will not repeat them.
[0054] Step 6, collecting iron phosphate, this step specifically includes:
[0055] Step 6.1, close the fifth valve V5, open the fourth valve V4 and the sixth valve V6, and transport the iron phosphate cleaned in step 5 to the dryer 6, where the dryer 6 dries the iron phosphate.
[0056] Step 6.2, collecting the iron phosphate dried by the dryer 6 into the storage tank 10.
[0057] The parts not specifically described in the above description are all prior art, or can be implemented by prior art. Moreover, the specific implementation cases described in the present invention are only preferred implementation cases of the present invention, and are not used to limit the scope of implementation of the present invention. That is, all equivalent changes and modifications made according to the content of the patent scope of the present invention should be regarded as the technical scope of the present invention.
Claims
1. A processing device for extracting iron phosphate using phosphating slag, characterized in that: The invention comprises a solid-liquid separator (2), a phosphating slag pretreatment device (3), a solid-liquid separation and cleaning device (4), a high-pressure hydrothermal reactor (5), an acid storage tank (7), a drying machine (6) and a material storage tank (10); the solid-liquid separator (2) is used to separate the phosphating liquid and the phosphating slag generated during the phosphating process; the phosphating slag pretreatment device (3) is connected to the solid-liquid separator (2); phosphoric acid is added to the phosphating slag separated by the solid-liquid separator (2) in the phosphating slag pretreatment device (3), and the phosphating slag is heated and stirred in the phosphating slag pretreatment device (3) to obtain a solid-liquid mixed product of the phosphating slag and phosphoric acid; The solid-liquid separation and cleaning device (4) is connected to the phosphating slag pretreatment device (3) and is used to separate and clean the solid-liquid mixed product of the phosphating slag and phosphoric acid reacted in the phosphating slag pretreatment device (3); the high-pressure hydrothermal reactor (5) is connected to the solid-liquid separation and cleaning device (4) and is used to perform a hydrothermal reaction on the solid product cleaned and separated by the solid-liquid separation and cleaning device (4) after adding phosphoric acid, and transport the solid product after the hydrothermal reaction to the solid-liquid separation and cleaning device (4) for cleaning and separation to obtain iron phosphate. The acid storage tank (7) is used to store phosphoric acid. The phosphating slag pretreatment device (3) and the high-pressure hydrothermal reactor (5) are both connected to the acid storage tank (7). The acid storage tank (7) is used to provide phosphoric acid to the phosphating slag pretreatment device (3) and the high-pressure hydrothermal reactor (5) when in use. The dryer (6) is connected to the solid-liquid separation and cleaning device (4) and is used to dry the iron phosphate cleaned by the solid-liquid separation and cleaning device (4). The material storage tank (10) is connected to the dryer (6) and is used to store the dried iron phosphate.
2. The processing device for extracting iron phosphate using phosphating slag according to claim 1, characterized in that: The phosphating slag pretreatment device (3) is connected to the high-pressure hydrothermal reactor (5) via a fifth pipeline, a seventh valve (V7) and an eighth valve (V8) are provided on the fifth pipeline, the fifth pipeline is connected to the acid storage tank (7) via a sixth pipeline, and the connection between the sixth pipeline and the fifth pipeline is located between the seventh valve (V7) and the eighth valve (V8).
3. The processing device for extracting iron phosphate using phosphating slag according to claim 1, characterized in that: It also comprises a water tower (9), which is in communication with the solid-liquid separation and cleaning device (4) and is used to add cleaning water into the solid-liquid separation and cleaning device (4).
4. The processing device for extracting iron phosphate using phosphating slag according to claim 1, characterized in that: The phosphating slag pretreatment device (3) is connected to the solid-liquid separation and cleaning device (4) through a first pipeline, and a second valve (V2) and a third valve (V3) are arranged on the first pipeline. The solid-liquid separation and cleaning device (4) is connected to the high-pressure hydrothermal reactor (5) through a third pipeline, and a fourth valve (V4) and a fifth valve (V5) are arranged on the third pipeline. The high-pressure hydrothermal reactor (5) is connected to the first pipeline through a second pipeline, and the connecting portion between the second pipeline and the first pipeline is located between the second valve (V2) and the third valve (V3). The drying machine (6) is connected to the third pipeline through a fourth pipeline, and the connecting portion between the fourth pipeline and the third pipeline is located between the fourth valve (V4) and the fifth valve (V5). A sixth valve (V6) is arranged on the fourth pipeline.
5. The processing device for extracting iron phosphate using phosphating slag according to claim 1, characterized in that: It also comprises a liquid storage tank (8), which is in communication with the solid-liquid separation and cleaning device (4) and is used to store liquid cleaned by the solid-liquid separation and cleaning device (4).
6. The processing device for extracting iron phosphate using phosphating slag according to claim 1, characterized in that: The solid-liquid separation and cleaning device (4) comprises a base (401), a box body (406) is arranged on the upper part of the base (401), the box body (406) is divided into a separation chamber and a cleaning chamber by a partition (411), a feed inlet (410) is provided at the top of one end of the separation chamber, the separation chamber is communicated with the end of the cleaning chamber away from the feed inlet (410), a screw conveying device is arranged in the separation chamber, and is used to push the solid matter in the separation chamber toward the side away from the feed inlet (410) and drop it into the cleaning chamber, a liquid discharge port is arranged on the side of the bottom of the separation chamber close to the feed inlet (410), and is used to discharge the liquid matter in the separation chamber; a water inlet (412) is arranged on the upper part of the cleaning chamber close to the feed inlet (410), and is used to add water to the cleaning chamber; a stirring shaft for fixing a plurality of first stirring paddles (409) is arranged in the cleaning chamber, and is used to stir the water and solid matter in the cleaning chamber; the base (401) A rotating drum (418) is rotatably arranged at the lower part, and a solid phase outlet (421) and a liquid phase outlet (422) are respectively provided at two ends of the rotating drum (418). A first conveying shaft having a first spiral blade fixed thereto is rotatably arranged in the rotating drum (418). The first conveying shaft is a hollow structure. One end of the first conveying shaft is connected to the bottom of one end of the cleaning chamber by a rotary joint and a seventh pipeline. A material distribution port (420) is radially arranged on the first conveying shaft. The solid-liquid mixture in the cleaning chamber is transported to the first conveying shaft through the seventh pipeline and discharged into the rotating drum (418) through the material distribution port (420), wherein liquid objects flow to the liquid phase outlet (422) and are discharged from the rotating drum (418), and solid objects are pushed to the solid phase outlet (421) by the first spiral blade and are discharged from the rotating drum (418). A differential (404) is provided on the first conveying shaft for adjusting the rotation speed of the first conveying shaft to be smaller than the rotation speed of the rotating drum (418).
7. The processing device for extracting iron phosphate using phosphating slag according to claim 6, characterized in that: A first motor (417) is installed on one end of the seventh pipeline on the base (401), and the first motor (417) is connected to the rotating drum (418) by a transmission belt (416). An electrical control system (403) is arranged on the other end of the base (401), and one end of the stirring shaft and the screw conveying device are both connected to the electrical control system and driven to rotate by a second motor in the electrical control system.
8. A method for extracting iron phosphate using phosphating slag, characterized in that: The processing device for extracting iron phosphate using phosphating slag as claimed in any one of claims 1 to 7 comprises the following steps: Step 1, using a solid-liquid separator (2) to separate the phosphating liquid and phosphating slag produced during the phosphating process; Step 2, adding phosphoric acid to the phosphating slag separated in step 1 in the phosphating slag pretreatment device (3), and stirring at 60 to 80° C. for 4 to 6 hours to obtain a solid-liquid mixture; Step 3, performing solid-liquid separation on the solid-liquid mixture of step 2 in a solid-liquid separation and cleaning device (4), and cleaning the solid objects therein with water; Step 4, subjecting the solid object cleaned in step 3 to a hydrothermal reaction in a high-pressure hydrothermal reactor (5) to obtain iron phosphate; Step 5, washing the iron phosphate obtained in step 4 in a solid-liquid separation and washing device (4); Step 6, collecting iron phosphate.
9. The method for extracting iron phosphate using phosphating slag according to claim 8, characterized in that: In step 4, the reaction temperature in the high-pressure hydrothermal reactor (5) is 180-220° C., the pressure is 1.2-1.5 MPa, and the reaction time is 4-6 h.
10. The method for extracting iron phosphate using phosphating slag according to claim 8 or 9, characterized in that: Step 6 includes, Step 6.1, using a dryer to dry the iron phosphate; Step 6.2, collecting the dried iron phosphate into a storage tank (10).
Citation Information
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