Zirconium oxychloride waste liquid filtering device and filtering method

Abstract

The invention relates to the technical field of zirconium oxychloride waste liquid, and particularly discloses a zirconium oxychloride waste liquid filtering device and a filtering method. Comprising a shell, a liquid inlet pipe arranged on the shell, a liquid outlet pipe arranged at the bottom of the shell, a stirring rod arranged in the shell and a neutralization assembly which is opened along with a certain rotation frequency of the stirring rod and is provided with a pH monitor, and a neutralizer is arranged in the neutralization assembly. The device solves the problem of how to accurately control the amount of a neutralizing agent in the traditional zirconium oxychloride waste liquid treatment link.

Description

Technical Field

[0001] The present invention relates to the technical field of zirconium oxychloride waste liquid, and specifically discloses a zirconium oxychloride waste liquid filtering device and filtering method. Background Art

[0002] Zirconium oxychloride waste liquid is an acidic waste liquid generated during the production of zirconium oxychloride. Zirconium oxychloride is mainly composed of zircon sand, mainly zirconium silicate. Zirconium silicate is prepared by alkali fusion method and needs to undergo multiple crystallization, separation and washing during the production process. In this process, trace impurity elements in the raw materials such as scandium, rare earth, iron, titanium, uranium, thorium, etc. are gradually enriched in the crystallization mother liquor. The crystallization mother liquor is discharged: After the zirconium oxychloride crystals are precipitated, the remaining mother liquor cannot be directly recycled due to the accumulation of impurities and needs to be neutralized before discharge. The traditional treatment method is neutralization reaction: such as adding sodium hydroxide to adjust the pH and then separating the solid and liquid, discharging sodium chloride wastewater, and stacking the waste residue; China Publication No. CN211384024U discloses a zirconium oxychloride waste liquid filtering device, comprising a centrifugal pump, a delivery pipe, a connecting cylinder, an activated carbon bag and a transfer barrel, wherein the centrifugal pump and the transfer barrel are connected via a delivery pipe, wherein the delivery pipe is evenly provided with connecting cylinders with a bottom sealing arrangement, and the delivery pipe is fixedly connected to the middle of the side wall of the connecting cylinder, a cross limiting rod is provided at the communication port between the delivery pipe and the connecting cylinder, the connecting cylinder is filled with an activated carbon bag of a size adapted thereto, wherein the top opening of the connecting cylinder is sealed by a sealing cover, and a drain valve is further provided at the bottom end of the connecting cylinder, the end of the delivery pipe passes through the top end of the side wall of the transfer barrel and is bent downward, wherein an exhaust port is further provided on the cover plate at the top of the transfer barrel, and a sealing cover is provided on the top of the cover plate to cover the exhaust cover, and an exhaust pipe connected to an acid mist absorption tower is provided at the top of the sealing cover; The activated carbon bag absorbs impurities in the solution to filter it, thereby filtering the solution during transportation and reducing the time required for clarification after the solution is transported to the transfer barrel. At the same time, when the volatile acid gas in the solution in the transfer barrel is discharged through the exhaust port, the sealing cover can prevent the acid gas from escaping, and the acid gas is introduced into the acid mist absorption tower for treatment through the exhaust pipe, thereby solving the problem of unorganized emission of acid mist and improving the working environment. The above solution uses activated carbon to adsorb impurities in the zirconium oxychloride waste liquid, which is equivalent to the above solution acting on the physical purification of the mother liquor, and does not treat the chemical impurities in the mother liquor. Therefore, the above solution has certain flaws; Based on the traditional method of adding sodium hydroxide to achieve neutralization reaction, and then completing solid-liquid separation to achieve impurity separation, in practice, there are problems with the addition of sodium hydroxide: Excessive sodium hydroxide: The amount of precipitation is reduced or redissolved: Some metal hydroxides may be partially dissolved due to excessive alkalinity, especially amphoteric metals such as Th(OH)4, which may form soluble complexes under strong alkalinity, which will greatly affect the purity of the mother liquor; Increased turbidity of the solution: Some dissolved metal ions may re-enter the solution, causing turbidity in the supernatant; Insufficient sodium hydroxide: First, the critical pH for complete precipitation of metal ions is not reached, and the precipitation is incomplete: some metal ions (such as Sc 3 ⁺, rare earth elements, Th 4 ⁺) still remains in the solution, causing the waste liquid to turn yellow or turbid. The most critical reason is that radioactive elements such as uranium (U) and thorium (Th) are not fully precipitated, which may cause environmental pollution after discharge; The current existing operation is: because the volume of the mother liquor generated each time is quantified, the amount of sodium hydroxide is matched according to the volume of the mother liquor each time, and then all the sodium hydroxide is added to the mother liquor to complete the neutralization reaction. This operation is not rigorous enough. Although the quantitative mother liquor volume can be matched to the amount of sodium hydroxide to achieve a small difference, the trace impurities in the mother liquor come from the trace impurities in the raw materials. The trace impurities in the raw materials do not have the same or similar content in each batch of raw materials. Therefore, the use of the conventional means mentioned above will inevitably lead to the adverse effects of insufficient or excessive sodium hydroxide on the mother liquor. In view of this, the inventors provide a zirconium oxychloride waste liquid filtration device and filtration method to solve the above problems. Summary of the Invention

[0003] The purpose of the present invention is to solve the problem of how to accurately control the amount of neutralizing agent in the traditional zirconium oxychloride waste liquid treatment process.

[0004] In order to achieve the above object, the present invention provides the following basic scheme: A zirconium oxychloride waste liquid filtering device comprises a shell, a liquid inlet pipe arranged on the shell, a liquid outlet pipe arranged at the bottom of the shell, a stirring rod arranged inside the shell, and a neutralization component with a pH monitor that opens when the stirring rod rotates at a certain frequency, and the neutralization component has a built-in neutralizer.

[0005] Furthermore, the neutralizing agent is sodium hydroxide solution.

[0006] Furthermore, the stirring rod is a hollow structure, one end of the stirring rod passes through the shell and is connected to the driving component, and the other end of the stirring rod is rotatably connected to the inner bottom of the shell.

[0007] Furthermore, the driving component is a motor, one end of the stirring rod is clamped with the motor output shaft, a groove connecting block is fixed to the inner bottom of the shell, a connecting bearing is provided inside the groove connecting block, the inner ring of the connecting bearing is connected to the other end of the stirring rod, and a rotating bearing is provided at the connection between the stirring rod passing through the shell and the shell.

[0008] Furthermore, the rotating bearing and the connecting bearing are both deep groove ball bearings.

[0009] Furthermore, the neutralization assembly includes hollow protrusions arranged on both sides of the stirring rod from top to bottom and connected to the stirring rod, a connecting block arranged at the connection between the hollow protrusion and the stirring rod, a spring installed on the connecting block, and a sealing block arranged at the free end of the spring, and the sealing block is installed at the end of the hollow protrusion.

[0010] Furthermore, one end of the spring is fixedly mounted on the connecting block, and the other end of the spring is connected to the sealing block. When the sealing block is mounted on the end of the hollow protrusion, the spring is in a normal state, and an outflow hole for the outflow of the neutralizer is provided at the center of the connecting block.

[0011] Furthermore, the elastic coefficients of the springs are all different, and the elastic coefficients of the springs increase sequentially along the direction of the inner bottom of the shell, and the internal volumes of the hollow protrusion and the stirring rod are determined.

[0012] Based on a zirconium oxychloride waste liquid filtering device, the present application also discloses a filtering method of the zirconium oxychloride waste liquid filtering device, comprising the following steps: S01: Manually inject the neutralizing agent through the hollow protrusion and the stirring rod, install the stirring rod and the housing in the housing, and wait for the mother liquid to be injected; S02: The mother liquor enters the shell through the liquid inlet pipe and accumulates. The motor starts at a low speed, and the mother liquor is in a dynamic state. At this time, the neutralization component is not opened. The motor speed is increased, the neutralization component is opened, and the data of the pH monitor is observed. S03: Based on the data from the pH monitor, increase or decrease the speed of the motor, and then constantly monitor the data from the pH monitor; S04: After the neutralization reaction, the mother liquor after the reaction is discharged through the liquid outlet pipe, and the waste residue remains in the shell and is subsequently cleaned.

[0013] Furthermore, it was observed that when the data from the pH monitor could not reach the alkaline environment, the motor speed reached the rated speed, and at this time all the neutralization components were opened.

[0014] The principle and effect of this solution are: 1. Compared with the prior art, the device has simple structure and ingenious design, the core of which is the adoption of a pH monitor and a neutralizing assembly, the neutralizing assembly is opened based on centrifugal force, the opening or closing of the neutralizing assembly is realized by rotating speed being above or below a threshold value, then whether the addition of the neutralizing agent is excessive or insufficient is judged according to the pH value monitored by the pH monitor, and when the reasonable pH value range of the pH monitor is reached, the device can still complete the stirring work and no longer release the neutralizing agent, the filtration of the mother liquor is completed by stirring acceleration, the waste residue is precipitated after the neutralization reaction, and then the filtration of the mother liquor is realized. BRIEF DESCRIPTION OF DRAWINGS

[0015] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiment description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without any creative effort on the basis of these drawings.

[0016] Figure 1 The structure schematic diagram of the zirconium oxychloride waste liquid filtration device proposed in the embodiment of the present application is shown; Figure 2 The front view schematic diagram of the zirconium oxychloride waste liquid filtration device proposed in the embodiment of the present application is shown; Figure 3 The cross-sectional schematic diagram of the neutralizing assembly in the zirconium oxychloride waste liquid filtration device proposed in the embodiment of the present application is shown; Figure 4 The structure schematic diagram of the communication block in the zirconium oxychloride waste liquid filtration device proposed in the embodiment of the present application is shown; Figure 5 The installation position schematic diagram of the spring in the zirconium oxychloride waste liquid filtration device proposed in the embodiment of the present application is shown. DETAILED DESCRIPTION

[0017] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined invention purpose, the specific embodiments, structures, features and effects according to the present application will be described in detail below in combination with the drawings and preferred embodiments.

[0018] The reference signs in the drawings of the specification include: end cover 1, liquid inlet pipe 2, motor 3, clamping part 4, rotating bearing 5, digital display instrument 6, shell 7, liquid outlet pipe 8, inclined surface 9, groove connecting block 10, stirring rod 11, hollow convex part 12, sealing block 13, activated carbon layer 14, spring 15, pH monitor 16, connecting block 17, communication block 18, installation ring groove 19, outflow hole 20.

[0019] The embodiments are as follows: Figure 1-Figure 5 as shown: A zirconium oxychloride waste liquid filtering device comprises a housing 7 and an end cap 1 provided on the housing 7, a liquid inlet pipe 2 provided on the housing 7, a liquid outlet pipe 8 provided at the bottom of the housing 7, a stirring rod 11 provided inside the housing 7, and a neutralization component with a pH monitor 16 that is opened when the stirring rod 11 rotates at a certain frequency, wherein the neutralization component has a built-in neutralizer.

[0020] Structurally, the liquid inlet pipe 2 is connected to the mother liquid discharge port. After the mother liquid discharge port is connected to the liquid inlet pipe 2, the mother liquid enters the shell 7. A switch valve is provided on the liquid outlet pipe 8. The switch valve is a mechanical switch valve. The liquid outlet pipe 8 is opened or closed by the switch valve. A filter is provided inside the liquid outlet pipe 8. Since the present application adopts a neutralization reaction to achieve mother liquid filtration, solid waste residue will be generated. The solid waste residue is blocked by the filter to achieve solid-liquid separation. In order to facilitate the cleaning of the waste residue, the liquid outlet pipe 8 is threadedly connected to the bottom of the shell 7. When the waste residue needs to be cleaned, the liquid outlet pipe 8 needs to be disassembled to collect and process the waste residue. The bottom of the shell 7 is provided with an inclined surface 9, which is used to accelerate the outflow of the mother liquid.

[0021] like Figure 3 As shown, the stirring rod 11 is a hollow structure, one end of the stirring rod 11 passes through the shell 7 and is connected to a drive component, and the other end of the stirring rod 11 is rotatably connected to the inner bottom of the shell 7. Specifically: the drive component is a motor 3, and the upper end of the stirring rod 11 is clamped with the output shaft of the motor 3. A clamping part 4 is provided at the clamping point between the upper end of the stirring rod 11 and the output shaft of the motor 3 for connecting the output shaft of the motor 3, and an activated carbon layer 14 is provided inside the clamping part 4. The practical activated carbon layer 14 adsorbs non-effective impurities in the neutralizer, and a groove connecting block 10 is fixed to the inner bottom of the shell 7, and a connecting bearing is provided inside the groove connecting block 10. The inner ring of the connecting bearing is connected to the lower end of the stirring rod 11, and a rotating bearing 5 is provided at the connection between the stirring rod 11 passing through the shell 7 and the shell 7. The rotating bearing 5 and the connecting bearing are both deep groove ball bearings.

[0022] The neutralization assembly includes, from top to bottom, a hollow protrusion 12 which is arranged on both sides of the stirring rod 11 and connected to the stirring rod 11, a connecting block 18 which is arranged at the connection between the hollow protrusion 12 and the stirring rod 11, a spring 15 installed on the connecting block 18, and a sealing block 13 arranged at the free end of the spring 15. The sealing block 13 is installed at the end of the hollow protrusion 12, one end of the spring 15 is fixedly installed on the connecting block 18, and the other end of the spring 15 is connected to the sealing block 13. When the sealing block 13 is installed at the end of the hollow protrusion 12, the spring 15 is in a normal state. An outflow hole 20 for the outflow of the neutralizer is provided in the center of the connecting block 18, and a mounting ring groove 19 is provided on the connecting block 18. The mounting ring groove 19 is used to install the spring 15.

[0023] Specifically: glue is provided at the connection between the sealing block 13 and the end of the hollow protrusion 12. The purpose of the glue is to prevent the neutralizer from flowing out from the connection between the sealing block 13 and the end of the hollow protrusion 12. The neutralizer in this application is sodium hydroxide solution.

[0024] Regarding the spring 15 : The elastic coefficients of the springs 15 are all different, and the elastic coefficients of the springs 15 increase sequentially along the direction of the inner bottom of the shell 7 , and are determined by the internal volumes of the hollow protrusion 12 and the stirring rod 11 .

[0025] When the present invention is used, a pH monitor is provided at the bottom of the stirring rod 11, and a digital display 6 is provided on the outside of the housing 7 for displaying the value of the pH monitor. The neutralizer is preferentially injected into the stirring rod 11. Since the hollow protrusion 12 and the internal volume of the stirring rod 11 are determined, the amount of the neutralizer injected can be known. Then, the bottom of the stirring rod 11 is formed into a connecting block 17, and the connecting block 17 is mounted on the groove connecting block 10. The top of the stirring rod 11 is connected to the output shaft of the motor 3. At this time, when the motor 3 is not started, the hollow protrusion 12 and the stirring rod 11 are a sealed environment. Then install the device, the mother liquid enters the shell 7, and the mother liquid enters the shell 7 through the liquid inlet pipe 2 and accumulates. The motor 3 is started at a low speed, the mother liquid is in a dynamic state, and the data of the pH monitor is observed. At this time, it is in a strong acid environment, and the neutralization component is not opened at this time; the motor 3 increases the speed, the neutralization component is opened, and the data of the pH monitor is observed. At this time, it should gradually enter a weak alkaline environment from a strong acid environment; The weak alkaline environment is 8-9 pH. Based on the data of the pH monitor, if the weak alkaline environment of 8-9 pH is not reached, the speed of the motor 3 needs to be increased. If the weak alkaline environment of 8-9 pH is reached too quickly, the speed of the motor 3 needs to be reduced to the low speed state of the motor 3. The data of the pH monitor is monitored at all times. When the speed of the motor 3 is increased, the centrifugal force overcomes the work of the spring 15, causing the sealing block 13 to move outward, thereby allowing the neutralizer inside the hollow protrusion 12 to flow out. When the speed of the motor 3 is reduced, the centrifugal force cannot overcome the work of the spring 15, the sealing block 13 returns to its original position, and the neutralizer no longer flows out. Since excessive impurity content will lead to a strong acid environment exceeding the standard, when it is observed that the data of the pH monitor cannot reach an alkaline environment within a certain period of time, the speed of motor 3 reaches the rated speed, and at this time all the neutralization components are opened, and the neutralizer is quickly added. Then the data of the pH monitor is observed, and if it is still acidic at this time, it is necessary to disassemble motor 3 and the output shaft of motor 3 and re-inject new neutralizer.

[0026] Finally, for the mother liquor, after the neutralization reaction, the mother body is filtered, and solid-liquid separation is realized through the filter screen. The device solves the problem of how to accurately control the amount of neutralizing agent in the traditional zirconium oxychloride waste liquid treatment link.

[0027] The above is only the preferred embodiment of the present application, and does not limit the present application in any form. Although the present application has been disclosed as above with the preferred embodiment, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical content to obtain equivalent embodiments with equivalent changes, without departing from the technical solution of the present application. Any modification, equivalent change and modification of the above embodiments made according to the technical essence of the present application, without departing from the technical solution of the present application, still belongs to the scope of the technical solution of the present application.

Claims

1. A zirconium oxychloride waste liquid filtering device, characterized in that: The invention comprises a shell, a liquid inlet pipe arranged on the shell, a liquid outlet pipe arranged at the bottom of the shell, a stirring rod arranged inside the shell, and a neutralization component with a pH monitor which opens as the stirring rod rotates at a certain frequency. The neutralization component has a built-in neutralizer.

2. A zirconium oxychloride waste liquid filtering device according to claim 1, characterized in that: The neutralizing agent is sodium hydroxide solution.

3. A zirconium oxychloride waste liquid filtering device according to claim 1 or 2, characterized in that: The stirring rod is a hollow structure. One end of the stirring rod passes through the shell and is connected to the driving component, and the other end of the stirring rod is rotatably connected to the inner bottom of the shell.

4. A zirconium oxychloride waste liquid filtering device according to claim 3, characterized in that: The driving component is a motor, one end of the stirring rod is clamped with the motor output shaft, a groove connecting block is fixed to the inner bottom of the shell, a connecting bearing is provided inside the groove connecting block, the inner ring of the connecting bearing is connected to the other end of the stirring rod, and a rotating bearing is provided at the connection between the stirring rod passing through the shell and the shell.

5. A zirconium oxychloride waste liquid filtering device according to claim 4, characterized in that: The rotating bearing and the connecting bearing are both deep groove ball bearings.

6. A zirconium oxychloride waste liquid filtering device according to claim 4, characterized in that: The neutralization assembly includes hollow protrusions arranged on both sides of the stirring rod from top to bottom and connected to the stirring rod, a connecting block arranged at the connection between the hollow protrusion and the stirring rod, a spring installed on the connecting block, and a sealing block arranged at the free end of the spring, and the sealing block is installed at the end of the hollow protrusion.

7. A zirconium oxychloride waste liquid filtering device according to claim 6, characterized in that: One end of the spring is fixedly mounted on the connecting block, and the other end of the spring is connected to the sealing block. When the sealing block is mounted on the end of the hollow protrusion, the spring is in a normal state. An outflow hole for the outflow of the neutralizer is provided at the center of the connecting block.

8. A zirconium oxychloride waste liquid filtering device according to claim 7, characterized in that: The elastic coefficients of the springs are all different, and the elastic coefficients of the springs increase sequentially along the direction of the inner bottom of the shell, and the internal volumes of the hollow protrusion and the stirring rod are determined.

9. A filtration method for a zirconium oxychloride waste liquid filtration device, for using the zirconium oxychloride waste liquid filtration device according to claim 8, characterized in that: The following steps are involved: S01: Manually inject the neutralizing agent through the hollow protrusion and the stirring rod, install the stirring rod and the housing in the housing, and wait for the mother liquid to be injected; S02: The mother liquor enters the shell through the liquid inlet pipe and accumulates. The motor starts at a low speed, and the mother liquor is in a dynamic state. At this time, the neutralization component is not opened. The motor speed is increased, the neutralization component is opened, and the data of the pH monitor is observed. S03: Based on the data from the pH monitor, increase or decrease the speed of the motor, and then constantly monitor the data from the pH monitor; S04: After the neutralization reaction, the mother liquor after the reaction is discharged through the liquid outlet pipe, and the waste residue remains in the shell, and the waste residue is cleaned up later.

10. The filtering method of a zirconium oxychloride waste liquid filtering device according to claim 9, characterized in that: When it is observed that the data from the pH monitor cannot reach the alkaline environment, the motor speed reaches the rated speed, and all the neutralization components are opened.

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