Impurity removing device for removing divalent ions from crude salt water for electrolysis

Abstract

The utility model discloses a kind of impurity removal treatment devices for removing divalent ion in electrolytic coarse salt water.The device for removing divalent ion in electrolytic coarse salt water includes: reactor main body, reactor main body has reaction cavity inside;M electrically conductive support nets, m electrically conductive support nets are set along the axial direction interval of reaction cavity, m electrically conductive support nets divide reaction cavity into (m+1) mixed reaction zones, when any two electrically conductive support nets are connected to power supply, electric field is formed between the two electrically conductive support nets, fluid inlet, fluid outlet, n reaction agent adding port are further provided on reactor main body, fluid inlet is directly communicated with the 1st mixed reaction zone, fluid outlet is directly communicated with the (m+1)th mixed reaction zone, and each reaction agent adding port is directly communicated with a mixed reaction zone.The utility model process is simple, safe and environmentally friendly, low in cost, and difficult to operate, and the device for removing divalent ion in electrolytic coarse salt water provided by the utility model has significant divalent ion removal rate advantage and performance stability.

Description

Technical Field

[0001] This utility model specifically relates to a purification treatment device for removing divalent ions from crude brine used in electrolysis, belonging to the fields of ion removal and environmental protection technology. Background Technology

[0002] Currently, domestic and international peers in the chlor-alkali industry are actively researching ways to reduce the concentration of divalent ions (CaO) in the brine used in chlor-alkali production. 2+ Mg 2+ Ba 2+ SO4 2- Methods for determining the content of divalent ions in brine. To enable the rapid development of the chlor-alkali industry to meet the demands of market economic development and satisfy existing raw material requirements, technological transformation and optimization are essential to improve product quality and stability. The quality of brine is crucial for achieving high yield and quality in chlor-alkali electrolysis production, resulting in optimal economic benefits. Furthermore, the divalent ions in the brine can affect other control data and the lifespan, yield, electrical efficiency, and power consumption of the electrolyzer's ion-exchange membrane.

[0003] The quality of brine is primarily determined by the controllability of divalent ion content. For many years, the brine refining process in my country's chlor-alkali industry has remained unchanged, relying on the traditional chemical precipitation method of treating electrolytic brine with barium chloride, sodium hydroxide, and sodium carbonate. Currently, the brine from the Kelvin membrane filter after treatment with sodium hydroxide and sodium carbonate has a high divalent cation content, averaging around 750 ppb, resulting in poor brine quality. This increases the load on divalent ions in the chelating resin tower in subsequent processes, thereby shortening the regeneration cycle of the chelating resin tower, increasing the number of regeneration cycles, and the discharge of regenerated acid, alkali, pure water, and wastewater. It also shortens the lifespan of the ion exchange membrane, thus increasing production costs.

[0004] Currently, the industry mainly adopts the following devices and treatment methods for removing divalent ions from crude brine used in electrolysis:

[0005] CN212050903U discloses a device for electrolytically treating sodium sulfate using a bipolar membrane electrodialysis system. This device utilizes bipolar membrane electrodialysis to electrolyze sodium sulfate. Since sulfuric acid and sodium hydroxide are essential raw materials for viscose fiber enterprises, sulfate and sodium ions can be recycled. This not only reduces production costs for enterprises but also alleviates the environmental pressure of solid waste treatment and the sales pressure of sodium sulfate. It solves the technical problem of the lack of an effective method for treating sodium sulfate in existing technologies. CN104030485A discloses an apparatus and method for removing divalent ions from crude brine used in electrolysis. The apparatus first removes a large amount of calcium and magnesium ions from the crude brine using sodium carbonate, and then further removes calcium and magnesium ions from the crude brine using phosphoric acid, utilizing the principle that calcium phosphate has a smaller Ksp than calcium carbonate. The total calcium and magnesium ion content in the crude brine exiting the chelating membrane filter is significantly lower than that in existing chelating membrane filters, thereby improving brine quality, reducing the reaction load on the chelating resin tower in subsequent processes, extending the regeneration cycle of the chelating resin tower, reducing the number of regeneration cycles, reducing the discharge of regenerated acid, alkali, pure water, and wastewater, extending the service life of the ion exchange membrane, and thus reducing production costs. CN205347592U discloses a device for decomposing chlorate in dilute brine for electrolysis. The device has a reasonable and compact structure, is easy to use, and achieves a high decomposition rate for chlorate in dilute brine. It can effectively reduce the chlorate content on the brine system side, greatly reducing the cost of subsequent processes and extending the service life of the ion exchange membrane. Furthermore, it significantly improves the quality of the brine, effectively reduces equipment investment, and does not affect the pressure of chlorine and hydrogen.

[0006] However, the currently disclosed devices and processes for removing divalent ions from crude brine used in electrolysis are lengthy, cumbersome, and difficult to operate. The resulting crude brine solution has a high content of divalent ions, especially the total content of calcium and magnesium ions, which averages around 750 ppb. The removal rate is low and unstable. Utility Model Content

[0007] To address the low removal rate of divalent ions in existing crude brine treatments for electrolysis, this invention, considering the properties of crude brine, process principles, and equipment structure, provides a device and method for removing divalent ions from crude brine used in electrolysis. This method, employing a segmented reaction device, overcomes the problems of lengthy, cumbersome, and difficult-to-operate treatment devices in existing technologies. It breaks through the main bottleneck in the effective removal of divalent ions from crude brine used in electrolysis, providing strong support for the industrialization of crude brine technology for electrolysis and thus overcoming the shortcomings of existing technologies.

[0008] To achieve the aforementioned objectives, the technical solution adopted by this utility model includes:

[0009] The first aspect of this utility model provides a purification device for removing divalent ions from crude brine used in electrolysis, comprising:

[0010] A reactor body, wherein the reactor body has a reaction chamber;

[0011] m conductive support meshes are disposed inside the reaction chamber and allow coarse brine to pass through. The m conductive support meshes are spaced apart along the axial direction of the reaction chamber, and the m conductive support meshes divide the reaction chamber into (m+1) mixing reaction zones. When any two conductive support meshes are connected to a power source, an electric field is formed between the two conductive support meshes, and the mixing reaction zone located between the two conductive support meshes is in the electric field.

[0012] Furthermore, the reactor body is also provided with a fluid inlet, a fluid outlet, and n reactant addition ports. The fluid inlet is directly connected to the first mixing reaction zone, the fluid outlet is directly connected to the (m+1)th mixing reaction zone, and each reactant addition port is directly connected to one of the mixing reaction zones, where m≥2 and n≥1.

[0013] A second aspect of this utility model provides a method for removing divalent ions from crude brine used in electrolysis, comprising:

[0014] A mixed reaction system is formed by mixing a crude brine solution containing divalent ions (including Ca2+) with a reactant solution. 2+ Ma 2+ Ba 2+ The reactant solution contains OH - and PO4 3- And, an electric field is applied to the mixed reaction system, wherein Ca in the mixed reaction system 2+ Ba 2+ With PO4 3- The reaction forms Ca3(PO4)2 precipitate, Ba3(PO4)2 precipitate, and Mg... 2 + With PO4 3- The reaction forms a precipitate of Mg3(PO4)2.

[0015] Compared with the prior art, the advantages of this utility model include:

[0016] This utility model provides a purification device for removing divalent ions from crude brine used in electrolysis. It utilizes a segmented reaction device to remove divalent ions from crude brine containing divalent ions, which can effectively improve the removal rate of divalent ions, greatly shorten the reaction time, and save water consumption.

[0017] The impurity removal method provided in this embodiment of the invention has a simple process flow, is safe and environmentally friendly, has low cost and low operation difficulty. Compared with the current devices for removing divalent ions from crude brine used in electrolysis, the device for removing divalent ions from crude brine used in electrolysis has a significant advantage in divalent ion removal rate and performance stability.

[0018] This utility model provides a purification device for removing divalent ions from crude brine used in electrolysis. The brine produced has excellent quality, reduces the reaction load on the chelating resin tower in subsequent processes, thereby extending the regeneration cycle of the chelating resin tower, reducing the number of regenerations of the chelating resin tower and the amount of regenerated acid, alkali, pure water and wastewater discharged, extending the service life of the ion exchange membrane, and thus reducing production costs. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the structure of a purification device for removing divalent ions from crude brine used in electrolysis, provided in a typical embodiment of this utility model.

[0020] Figure 2 yes Figure 1 Enlarged view of the structure Z in the middle;

[0021] Figure 3 This is a top view of a purification device for removing divalent ions from crude brine used in electrolysis, provided in a typical embodiment of this utility model. Detailed Implementation

[0022] In view of the shortcomings of the prior art, the inventor of this case, through long-term research and extensive practice, has come up with the technical solution of this utility model. The following will further explain the technical solution, its implementation process, and its principles.

[0023] This invention provides a purification device for removing divalent ions from crude brine used in electrolysis. Through multiple experiments and improvements, the device has been continuously optimized and improved in terms of the reaction time between the reactant and divalent ions, the pH value of the reaction solution (the pH value of the mixed reaction system in this invention is about 7), and the concentration of the reactant. This has resulted in a highly efficient purification device for removing divalent ions from crude brine used in electrolysis. It ensures efficient removal of divalent ions from the crude brine while significantly reducing the reaction time, making an outstanding contribution to the purification of crude brine in the electrolysis industry.

[0024] The first aspect of this utility model provides a purification device for removing divalent ions from crude brine used in electrolysis, comprising:

[0025] A reactor body, wherein the reactor body has a reaction chamber;

[0026] m conductive support meshes are disposed inside the reaction chamber and allow coarse brine to pass through. The m conductive support meshes are spaced apart along the axial direction of the reaction chamber, and the m conductive support meshes divide the reaction chamber into (m+1) mixing reaction zones. When any two conductive support meshes are connected to a power source, an electric field is formed between the two conductive support meshes, and the mixing reaction zone located between the two conductive support meshes is in the electric field.

[0027] Furthermore, the reactor body is also provided with a fluid inlet, a fluid outlet, and n reactant addition ports. The fluid inlet is directly connected to the first mixing reaction zone, the fluid outlet is directly connected to the (m+1)th mixing reaction zone, and each reactant addition port is directly connected to one of the mixing reaction zones, where m≥2 and n≥1.

[0028] Furthermore, the conductive support mesh is fixedly connected to the reactor body and sealed together.

[0029] Furthermore, a sealing ring is provided between the conductive support mesh and the reactor shell, and the two parts are sealed together via the sealing ring.

[0030] Furthermore, the reactor body includes (m+1) reactor shell segments, which are sequentially arranged along their own axial direction. m conductive support meshes are respectively arranged between the (m+1) reactor shell segments. The conductive support meshes are fixed and sealed to the reactor shells. The first reactor shell segment and the first conductive support mesh, the (m+1) reactor shell segment and the m-th conductive support mesh, the x-th reactor shell segment and the y-th and (y+1)-th conductive support meshes respectively enclose a mixing reaction zone. The first reactor shell segment serves as the upper cover, and the (m+1)-th reactor shell segment serves as the lower cover. The fluid inlet is located on the first reactor shell segment, the fluid outlet is located on the (m+1)-th reactor shell segment, and the reactant addition port is located on any of the reactor shell segments, where 1 ≤ x ≤ (m+1) and 1 ≤ y ≤ m.

[0031] Furthermore, the conductive support mesh is fixedly connected to the reactor shell via a conductive threaded connection assembly. The conductive support mesh is electrically connected to the threaded connection assembly and is also electrically connected to a power source via the threaded connection assembly.

[0032] Furthermore, the pore size / porosity of the conductive support mesh is 5 mesh to 100 mesh.

[0033] Furthermore, the end of the reactor shell has a fixed platform extending outward in its own radial direction, and the sealing ring is disposed at least between the fixed platform and the conductive support mesh. The fixed platform is fixedly connected to the conductive support mesh via the threaded connection assembly.

[0034] Furthermore, two fixed platforms located on the upper and lower sides of the conductive support net are defined as a first fixed platform and a second fixed platform, respectively. The first fixed platform is located above the conductive support net, and the radial width of the first fixed platform is greater than the radial width of the second fixed platform. The first fixed platform is fixedly connected to the conductive support net and the second fixed platform via a first threaded connection assembly. The first fixed platform is also fixedly connected to the conductive support net via a second threaded connection assembly. The second connection assembly is arranged radially on the outside of the second fixed platform along the reactor shell.

[0035] In a typical implementation, the impurity removal device for removing divalent ions from crude brine used for electrolysis further includes: m filter screens, each of which is covered by a conductive support mesh and is used at least to filter precipitates and suspended solids.

[0036] Furthermore, the filter screen is axially covered on the lower surface of the conductive support mesh.

[0037] Furthermore, the impurity removal device for removing divalent ions from crude brine used in electrolysis also includes a power source, which is electrically connected to the conductive support network.

[0038] Furthermore, the power supply is a DC power supply with a voltage of 3V to 6V.

[0039] A second aspect of this utility model provides a method for removing divalent ions from crude brine used in electrolysis, comprising:

[0040] A mixed reaction system is formed by mixing a crude brine solution containing divalent ions (including Ca2+) with a reactant solution. 2+ Ma 2+ Ba 2+ The reactant solution contains OH - and PO4 3- And, an electric field is applied to the mixed reaction system, wherein Ca in the mixed reaction system 2+ Ba 2+ With PO4 3- The reaction forms Ca3(PO4)2 precipitate, Ba3(PO4)2 precipitate, and Mg... 2 + With PO4 3- The reaction forms a precipitate of Mg3(PO4)2.

[0041] Furthermore, the method for removing divalent ions from the crude brine used for electrolysis specifically includes: reacting the crude brine containing divalent ions with a first reactant solution containing OH- and a solution containing PO4-. 3-The second reactant solution is mixed to form the mixed reaction system.

[0042] Furthermore, the concentration of OH- in the first reactant solution is 5wt% to 20wt%, and the concentration of PO4 in the second reactant solution is... 3- The concentration is 10wt% to 30wt%.

[0043] Furthermore, the crude brine containing divalent ions for electrolysis is mixed with the reactant solution in a flowing state.

[0044] Furthermore, the flow rate of the crude brine containing divalent ions for electrolysis is 200 mL / h to 500 mL / h.

[0045] Furthermore, the crude brine containing divalent ions is used in electrolysis with OH- ions. - The first reactant solution, containing PO4 3- The volume ratio or mass ratio of the second reactant solution is (200000~500000):3:1.

[0046] Furthermore, the electric field strength of the electric field is 200V / m to 400V / m.

[0047] Furthermore, the first reactant solution is a sodium hydroxide solution, and the second reactant solution is a phosphoric acid solution.

[0048] Furthermore, the method for removing divalent ions from crude brine used for electrolysis is implemented based on the impurity removal treatment device for removing divalent ions from crude brine used for electrolysis.

[0049] Furthermore, the method specifically includes: introducing crude brine for electrolysis into the reaction chamber through the fluid inlet, and sequentially entering (m+1) mixing reaction zones; adding the reactant solution into the mixing reaction zone through the reactant addition port; and connecting the conductive support mesh to a power source to form the electric field.

[0050] The following will provide a further explanation of the technical solution, its implementation process, and its principles, in conjunction with the accompanying drawings and specific implementation examples.

[0051] In a typical embodiment, a purification device for removing divalent ions from crude brine used in electrolysis includes a reactor body 44 and m conductive support meshes. The reactor body 44 has a reaction chamber. The m conductive support meshes are disposed in the reaction chamber and can be permeated by the crude brine. The m conductive support meshes are spaced apart along the axial direction of the reaction chamber, dividing the reaction chamber into (m+1) mixing reaction zones. The reactor body 4 is also provided with a fluid inlet 1, a fluid outlet 6, and n reactant addition ports 3. The fluid inlet 1 is directly connected to the first mixing reaction zone, the fluid outlet 6 is directly connected to the (m+1)th mixing reaction zone, and each reactant addition port 3 is directly connected to one of the mixing reaction zones, where m≥2 and n≥1. The conductive support meshes can be electrically connected to an external power source. When any two of the conductive support meshes are connected to a power source, an electric field is formed between the two conductive support meshes, and the mixing reaction zone located between the two conductive support meshes is in the electric field.

[0052] The conductive support mesh 5 is connected to the negative terminal of the power supply, and the conductive support mesh 14 is connected to the positive terminal of the power supply. The lower surface of the conductive support mesh 14 is attached with a filter screen to filter out sediment and suspended matter.

[0053] Specifically, the reaction chamber is sealed externally, and (m+1) mixing reaction zones are arranged sequentially along the axial direction. The crude brine for electrolysis, input from fluid inlet 1, can pass through the conductive support mesh and flow sequentially through the (m+1) mixing reaction zones. Specifically, the pore size / porosity of the conductive support mesh is 5 mesh to 100 mesh. It is understood that the mixing reaction zones / reaction chamber are used to contain the mixed reaction system including the crude brine for electrolysis and the reactant, to provide the mixed reaction system for the removal of divalent ions, and to provide the reaction conditions required for the mixed reaction system to undergo the reaction. It should be noted that fluid inlet 1, fluid outlet 6, and reactant addition port 3 can all be interfaces known in the art, which can be opened and closed.

[0054] Of course, observation windows for observing the reaction inside the mixing reaction zone can also be provided on the reactor body 4. Additionally, auxiliary mechanisms such as level gauges, temperature sensors, and pressure sensors can be installed inside the reactor body 4. The level gauge monitors the liquid level inside the reaction chamber, the temperature sensor monitors the temperature of the mixed reaction system inside the reaction chamber, and the pressure sensor monitors the pressure inside the reaction chamber. Similarly, pressure relief valves can also be installed on the reactor body 4. It should be noted that level gauges, temperature sensors, pressure sensors, and pressure relief valves are all known in the art, and their functions here are the same as those known in the art; therefore, their specific installation locations and assembly structures are not limited here.

[0055] Specifically, in order to facilitate the replacement of the reactant, at least one reactant replacement port 12 can be provided on the reactor body 4. The reactant replacement port 12 is connected to the mixing reaction zone. Specifically, in the axial direction of the reactor body 4, the reactant replacement port 12 is located above the conductive support mesh, and its axial position is slightly higher than the axial position of the conductive support mesh.

[0056] Specifically, the outer periphery of the conductive support mesh is fixedly connected to and sealed to the reactor body 4. More specifically, a sealing ring is provided between the conductive support mesh and the reactor shell, and the two parts are sealed together via the sealing ring.

[0057] Specifically, in order to enable the conductive support mesh to be connected to an external power source and to realize segmented (m+1) mixing reaction zones, the reactor body 4 includes (m+1) reactor shell sections (the reactor shell can be a hollow column / cylindrical structure; therefore, each reactor shell section can be called a reaction column or reaction cylinder, the same below). The (m+1) reactor shell sections are arranged sequentially along their own axial direction, and m conductive support meshes are respectively arranged between the (m+1) reactor shell sections. The conductive support meshes are fixed and sealed to the reactor shells. The first reactor shell section... The reactor body and the first conductive support mesh, the (m+1)th reactor shell and the mth conductive support mesh, the xth reactor shell and the yth and (y+1)th conductive support meshes respectively enclose a mixing reaction zone, wherein the first reactor shell serves as the upper cover 2, the (m+1)th reactor shell serves as the lower cover 13, the fluid inlet 1 is located on the first reactor shell, the fluid outlet 6 is located on the (m+1)th reactor shell, and the reactant addition port 3 is located on any of the reactor shells, 1≤x≤(m+1), 1≤y≤m.

[0058] It should be noted that although the reactor body 4 is divided into (m+1) mixing reaction zones, those skilled in the art can arbitrarily select any number of these mixing reaction zones as the main areas where the actual reaction occurs, and connect them to a power source through any two conductive support grids to form an electric field. Generally, the first and (m+1)th mixing reaction zones are not considered as the main areas where the mixing reaction occurs; that is, the reactant is mainly added directly to the mixing reaction zone located between the two ends.

[0059] Specifically, the first reactor shell and the (m+1)th reactor shell are structures that are closed at one end and open at the other end. The reactor shell in the middle section is open at both ends. The (m+1)th reactor shell and the m conductive support meshes are alternately arranged along the axial direction. The upper and lower ends of the reactor body 4 are both reactor shells. The (m+1)th reactor shell and the m conductive support meshes together enclose and form a reaction chamber and (m+1) mixing reaction zones.

[0060] Specifically, the conductive support mesh extends along the radial section of the reactor body 4. The conductive support mesh is fixedly connected to the reactor shell through a conductive threaded connection assembly. The conductive support mesh is electrically connected to the threaded connection assembly and is electrically connected to the power source via the threaded connection assembly.

[0061] For example, Figure 1 The impurity removal device shown for removing divalent ions from crude brine used in electrolysis includes three conductive support meshes, namely a first conductive support mesh 14, a second conductive support mesh 5, and a third conductive support mesh 15. At least two mixing reaction zones are formed inside the reactor body 4, and the two mixing reaction zones are respectively located between the first conductive support mesh 14, the second conductive support mesh 5, and the third conductive support mesh 15.

[0062] Specifically, the reactor shell has a fixed platform extending outward in its radial direction at one end. The sealing ring is disposed at least between the fixed platform and the conductive support mesh. The fixed platform is fixedly connected to the conductive support mesh via a threaded connection assembly. More specifically, two fixed platforms located on the upper and lower sides of the conductive support mesh are defined as a first fixed platform and a second fixed platform. The first fixed platform is located above the conductive support mesh, and its radial width is greater than that of the second fixed platform. The first fixed platform is fixedly connected to the conductive support mesh and the second fixed platform via a first threaded connection assembly. The first fixed platform is also fixedly connected to the conductive support mesh via a second threaded connection assembly. The second connection assembly is disposed radially outside the second fixed platform. Please refer to [link to relevant documentation]. Figure 1 and Figure 2 Each conductive support mesh is fixedly connected to the reactor shell located on its upper and lower sides by at least two sets of threaded connection assemblies. Each set of threaded connection assemblies includes a first threaded connection assembly and a second threaded connection assembly, as is known in the art. The threaded connection assembly includes bolts / screws, nuts, and washers, etc.

[0063] For example, the first threaded connection assembly includes a first screw 7 and a first washer 8, and the second threaded connection assembly includes a first screw 10 and a first washer 9. It is known in the art that the screw and the washer work together to connect and fix the two structural components, and no particular limitation is made here.

[0064] Specifically, the impurity removal device for removing divalent ions from crude brine used in electrolysis may further include m filter screens, each of which covers a conductive support mesh and is used at least to filter precipitates and suspended solids. Specifically, the filter screens are axially disposed on the lower surface of the conductive support mesh. The filter screens can be fixed to the conductive support mesh in a manner known in the art. The filter screens must be able to filter precipitates formed in the mixed reaction system but allow the solution to pass through. Their specific porosity and material are not limited here.

[0065] Specifically, the impurity removal device for removing divalent ions from crude brine used in electrolysis further includes: a power source, which is electrically connected to the conductive support mesh. The power source is a DC power source with a voltage of 3V to 6V. Specifically, the conductive support mesh can be electrically connected to a threaded connection assembly, and the power source is electrically connected to the threaded connection assembly, that is, the power source is electrically connected to the conductive support mesh via the threaded connection assembly.

[0066] In a typical implementation scheme, the method for removing divalent ions from crude brine used for electrolysis using the aforementioned impurity removal treatment device specifically includes the following steps:

[0067] S1: Add sodium hydroxide solution (concentration 5wt%–20wt%) and industrially diluted phosphoric acid (concentration 10wt%–30wt%) to the mixed reaction zone through reactant addition port 3. The amounts of sodium hydroxide solution and phosphoric acid added are determined based on the assumption that the neutralization reaction between sodium hydroxide solution and phosphoric acid solution will completely produce sodium phosphate.

[0068] S2: The solution to be purified is crude brine containing divalent ions used in electrolysis, specifically brine used in chlor-alkali production. The divalent ions in this brine include Ca2+. 2+ Ma 2+ Ba 2+ The divalent ion content is 1000 ppb to 2000 ppb. Crude brine is introduced into the reaction chamber through fluid inlet 1 at a flow rate of 200 L / h to 500 L / h, and sequentially enters (m+1) mixing reaction zones. The crude brine, sodium hydroxide solution (concentration 5 wt% to 20 wt%), and industrially diluted phosphoric acid (concentration 10 wt% to 30 wt%) form a mixed reaction system. The Ca in the mixed reaction system... 2+ Ba 2+ With PO4 3- The reaction forms Ca3(PO4)2 precipitate, Ba3(PO4)2 precipitate, and Mg... 2+ With PO4 3- The reaction forms Mg3(PO4)2 precipitate, and the two reactants (sodium hydroxide solution and phosphoric acid solution) undergo a neutralization reaction to generate sodium phosphate. The reaction is stopped after 1 to 4 hours.

[0069] The divalent ion content in the crude brine used for electrolysis is not constant. The crude brine with a higher divalent ion content has a higher flow rate, while the brine with a lower content has a lower flow rate. This not only allows the divalent cations to react fully and form a precipitate, but also allows for different flow rates to be used according to different divalent ion contents, which can effectively shorten the reaction time, i.e., reduce the residence time of the brine in the device.

[0070] S3: Connect two adjacent conductive support grids to a DC power supply with a voltage of 3V to 6V to form an electric field in the mixing reaction zone between the two adjacent conductive support grids. The electric field strength is 200V / m to 400V / m. By increasing the electric field, cations can be promoted to move towards the cathode and anions to move towards the anode, promoting ion collisions and reactions to accelerate the precipitation rate.

[0071] S4: During the mixing reaction, pure water is introduced into the reaction chamber at a rate of 200 mL / h to 500 mL / h through fluid inlet 1 to quickly rinse the mixing reaction system. The introduction of pure water can keep the mixing reaction system in a state of continuous agitation, which accelerates the precipitation reaction between the reactant and divalent ions. The pure water is introduced for 2 hours, and the precipitate is blocked by the filter screen located at the bottom of the mixing reaction zone.

[0072] Example 1

[0073] The solution to be purified is a crude brine containing divalent ions, including Ca2+, used for electrolysis. 2+ Ma 2+ Ba 2+ The content of divalent ions is 1000 ppb.

[0074] Add 18 ml of 5 wt% sodium hydroxide solution (mass percentage concentration of 5%) and 6 ml of 10 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body.

[0075] The solution to be purified was introduced into the reactor body at a flow rate of 200 mL / h, and the feeding was stopped after 2 hours of reaction.

[0076] Pure water is introduced into the reactor body at a flow rate of 200 mL / h to keep the mixed reaction system in an agitated state, quickly rinse the reactants, and then carry out the precipitation reaction.

[0077] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 3V and maintain this voltage for 2 hours.

[0078] Example 2

[0079] The solution to be purified is a crude brine containing divalent ions, including Ca2+, used for electrolysis. 2+ Ma 2+ Ba 2+The content of divalent ions is 1000 ppb.

[0080] Add 24 ml of 10 wt% sodium hydroxide solution and 8 ml of 15 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body;

[0081] The solution to be purified was introduced into the reactor body at a flow rate of 250 mL / h, and the feeding was stopped after 2 hours of reaction.

[0082] Pure water is introduced into the reactor body at a flow rate of 200 mL / h;

[0083] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 3V and maintain this voltage for 2 hours.

[0084] Example 3

[0085] The solution to be purified is electrolyzed using crude brine containing divalent ions, including Ca2+. 2+ Ma 2+ Ba 2+ The content of divalent ions is 1000 ppb.

[0086] Add 18 ml of 10 wt% sodium hydroxide solution and 6 ml of 20 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body;

[0087] The solution to be purified was introduced into the reactor body at a flow rate of 300 mL / h, and the feeding was stopped after 3 hours of reaction.

[0088] Pure water is introduced into the reactor body at a flow rate of 200 mL / h to quickly rinse the reactants before precipitation reaction.

[0089] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 3V and maintain this voltage for 3 hours.

[0090] Example 4

[0091] The solution to be purified is a crude brine containing divalent ions, including Ca2+, used for electrolysis. 2+ Ma 2+ Ba 2+ The content of divalent ions is 1000 ppb.

[0092] Add 30 ml of 15 wt% sodium hydroxide solution and 10 ml of 20 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body;

[0093] The solution to be purified was introduced into the reactor body at a flow rate of 350 mL / h, and the feeding was stopped after 4 hours of reaction.

[0094] Pure water is introduced into the reactor body at a flow rate of 200 mL / h to quickly rinse the reactants before precipitation reaction.

[0095] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 4V and maintain this voltage for 4 hours.

[0096] Example 5

[0097] The solution to be purified is a crude brine containing divalent ions, including Ca2+, used for electrolysis. 2+ Ma 2+ Ba 2+ The content of divalent ions is 1000 ppb.

[0098] Add 33 ml of 20 wt% sodium hydroxide solution and 11 ml of 25 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body;

[0099] The solution to be purified was introduced into the reactor body at a flow rate of 400 mL / h, and the feeding was stopped after 4 hours of reaction.

[0100] Pure water is introduced into the reactor body at a flow rate of 200 mL / h to quickly rinse the reactants before precipitation reaction.

[0101] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 1V and maintain this voltage for 4 hours.

[0102] Example 6

[0103] The solution to be purified is a crude brine containing divalent ions, including Ca2+, used for electrolysis. 2+ Ma 2+ Ba 2+ The content of divalent ions is 1000 ppb.

[0104] Add 33 ml of 20 wt% sodium hydroxide solution and 11 ml of 30 wt% industrial phosphoric acid to the mixing reaction zone inside the reactor body;

[0105] The solution to be purified was introduced into the reactor body at a flow rate of 450 mL / h, and the feeding was stopped after 3 hours of reaction.

[0106] Pure water is introduced into the reactor body at a flow rate of 200 mL / h to quickly rinse the reactants before precipitation reaction.

[0107] Connect two adjacent conductive support meshes to an external DC power supply with a voltage of 2V and maintain this voltage for 3 hours.

[0108] Compare with Example 1

[0109] This comparative example is a parallel experiment based on Example 1, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 2 hours.

[0110] Compare with Example 2

[0111] This comparative example is a parallel experiment based on Example 2, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 2 hours.

[0112] Compare with Example 3

[0113] This comparative example is a parallel experiment based on Example 3, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 3 hours.

[0114] Compare with Example 4

[0115] This comparative example is a parallel experiment based on Example 4, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 4 hours.

[0116] Compare with Example 5

[0117] This comparative example is a parallel experiment based on Example 5, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 4 hours.

[0118] Compare with Example 6

[0119] This comparative example is a parallel experiment based on Example 6, in which no external DC power supply is connected during the precipitation reaction, and the precipitation reaction continues for 3 hours.

[0120] All examples and control examples were tested three times, and the average value was taken. The results are shown in the table below.

[0121]

[0122] Experiments have verified that adding reactants (phosphate and sodium hydroxide) to a segmented reaction apparatus allows crude brine containing divalent ions to flow through it, removing the divalent ions. With the aid of an external electric field, the reaction continues for 2–4 hours, and the removal rate of divalent ions is over 93%. Without an electric field, after 2–4 hours of continuous reaction, the removal rate of divalent ions by the reactants is over 90%. Clearly, the removal rate of divalent ions can be significantly improved by using an external electric field.

[0123] This invention provides a purification device for removing divalent ions from crude brine used in electrolysis. Utilizing a segmented reaction device, it effectively removes divalent ions from the crude brine, significantly improving the removal rate, greatly shortening the reaction time, and saving water consumption. The purification method provided by this invention is simple, safe, environmentally friendly, low-cost, and easy to operate. Compared with current devices for removing divalent ions from crude brine used in electrolysis, this device has a significant advantage in divalent ion removal rate and performance stability.

[0124] This utility model provides a purification device for removing divalent ions from crude brine used in electrolysis. The brine produced has excellent quality, reduces the reaction load on the chelating resin tower in subsequent processes, thereby extending the regeneration cycle of the chelating resin tower, reducing the number of regenerations of the chelating resin tower and the amount of regenerated acid, alkali, pure water and wastewater discharged, extending the service life of the ion exchange membrane, and thus reducing production costs.

[0125] It should be understood that the above embodiments are merely illustrative of the technical concept and features of this utility model, and are intended to enable those skilled in the art to understand the content of this utility model and implement it accordingly. They should not be construed as limiting the scope of protection of this utility model. All equivalent changes or modifications made in accordance with the spirit and essence of this utility model should be included within the scope of protection of this utility model.

Claims

1. A purification device for removing divalent ions from crude brine used in electrolysis, characterized in that, include: A reactor body, wherein the reactor body has a reaction chamber; m conductive support meshes are disposed inside the reaction chamber and allow coarse brine to pass through. The m conductive support meshes are spaced apart along the axial direction of the reaction chamber, and the m conductive support meshes divide the reaction chamber into (m+1) mixing reaction zones. When any two conductive support meshes are connected to a power source, an electric field is formed between the two conductive support meshes, and the mixing reaction zone located between the two conductive support meshes is in the electric field. Furthermore, the reactor body is also provided with a fluid inlet, a fluid outlet, and n reactant addition ports. The fluid inlet is directly connected to the first mixing reaction zone, the fluid outlet is directly connected to the (m+1)th mixing reaction zone, and each reactant addition port is directly connected to one of the mixing reaction zones, where m≥2 and n≥1.

2. The purification treatment device for removing divalent ions from crude brine for electrolysis according to claim 1, characterized in that: The conductive support mesh is fixedly connected to the reactor body and sealed together.

3. The impurity removal device for removing divalent ions from crude brine used in electrolysis according to claim 2, characterized in that: A sealing ring is provided between the conductive support mesh and the reactor shell, and the sealing mesh is sealed together.

4. The purification treatment device for removing divalent ions from crude brine for electrolysis according to claim 1 or 2, characterized in that: The reactor body comprises (m+1) reactor shell segments, which are sequentially arranged along their axial direction. m conductive support meshes are respectively arranged between the (m+1) reactor shell segments. The conductive support meshes are fixed and sealed to the reactor shells. The first reactor shell segment and the first conductive support mesh, the (m+1) reactor shell segment and the m-th conductive support mesh, the x-th reactor shell segment and the y-th and (y+1)-th conductive support meshes respectively enclose a mixing reaction zone. The first reactor shell segment serves as the upper cover, and the (m+1) reactor shell segment serves as the lower cover. The fluid inlet is located on the first reactor shell segment, the fluid outlet is located on the (m+1) reactor shell segment, and the reactant addition port is located on any of the reactor shell segments, where 1 ≤ x ≤ (m+1) and 1 ≤ y ≤ m.

5. The impurity removal device for removing divalent ions from crude brine for electrolysis according to claim 4, characterized in that: The conductive support mesh is fixedly connected to the reactor shell through a conductive threaded connection assembly. The conductive support mesh is electrically connected to the threaded connection assembly and is also electrically connected to the power source via the threaded connection assembly. And / or, the pore size / porosity of the conductive support mesh is 5 mesh to 100 mesh.

6. The impurity removal device for removing divalent ions from crude brine for electrolysis according to claim 5, characterized in that: The reactor shell has a fixed platform extending outward in its radial direction at its end. The sealing ring is disposed at least between the fixed platform and the conductive support mesh. The fixed platform is fixedly connected to the conductive support mesh via the threaded connection assembly.

7. The purification device for removing divalent ions from crude brine for electrolysis according to claim 6, characterized in that: Two fixed platforms located on the upper and lower sides of the conductive support net are defined as a first fixed platform and a second fixed platform. The first fixed platform is located above the conductive support net, and the radial width of the first fixed platform is greater than that of the second fixed platform. The first fixed platform is fixedly connected to the conductive support net and the second fixed platform via a first threaded connection assembly. The first fixed platform is also fixedly connected to the conductive support net via a second threaded connection assembly. The second connection assembly is arranged radially on the outside of the second fixed platform along the reactor shell.

8. The impurity removal device for removing divalent ions from crude brine for electrolysis according to claim 1, characterized in that, It also includes: m filter screens, each of which covers a conductive support mesh and is used at least for filtering sediment and suspended matter.

9. The impurity removal device for removing divalent ions from crude brine for electrolysis according to claim 8, characterized in that: The filter screen is axially covered on the lower surface of the conductive support mesh.

10. The impurity removal device for removing divalent ions from crude brine for electrolysis according to claim 1, characterized in that: The impurity removal device for removing divalent ions from crude brine used in electrolysis further includes: a power source, which is electrically connected to the conductive support network; And / or, the power supply is a DC power supply, and the voltage of the power supply is 3V to 6V.

Images