Filtering assembly, thickening separator and reaction thickening separation system and method

Abstract

The invention discloses a filter assembly, a thickening separator and a reaction thickening separation system and method.The reaction thickening separation system comprises a reaction kettle, a middle receiving tank, the thickening separator and a regenerated liquid preparation tank; the reaction kettle is used for fully mixing various materials according to certain components and promoting growth of crystals to obtain a solution containing the crystals; the middle receiving tank is used for storing the solution, preventing the solution from precipitating, providing pressure through a diaphragm pump and conveying the solution into the thickening separator; clear liquid and thick slurry are separated through a filtering assembly in the thickening separator, the clear liquid flows into a clear liquid tank, and the thick slurry returns to the reaction kettle; the regenerated liquid preparation tank is used for accurately proportioning regenerated liquid by utilizing a control system so as to clean and maintain a filter assembly in the thickening separator to be regenerated; according to the invention, efficient material mixing, crystal growth, solution concentration and automatic cleaning and maintenance of the filtering assembly are realized, so that the production efficiency and the product quality are improved.

Description

Technical Field

[0001] The invention relates to the technical field of preparation technology, and more particularly to a filtering component, a thickening separator, a reaction thickening separation system and a method. Background Art

[0002] With the rapid development of new energy, lithium battery and fine chemical industries, these fields have put forward more stringent requirements on solid-liquid separation technology in the production process. As a key solid-liquid separation equipment, thickener separator plays a vital role in the production process of these industries, which are characterized by processing high value-added products and have extremely high standards for production efficiency and product quality. Therefore, the design and performance of the thickener separator will directly affect the purity and production cost of the final product.

[0003] In these industries, traditional filtration technology often fails to meet the growing demand, especially when dealing with highly corrosive, viscous or fine solid particles. In order to meet these challenges, the filter elements required for thickener separators must have the following characteristics: high strength, high precision, corrosion resistance and long-term durability. These requirements have promoted the development of filtration technology and prompted the continuous innovation of thickener separator filter elements in material selection, structural design and surface treatment to meet the high-standard production requirements of new energy, lithium battery and fine chemical industries. Therefore, the research and development and optimization of thickener separator filter elements have become a key link in the technological progress of these industries. Summary of the invention

[0004] The object of the present invention is to provide a filtering component, a thickening separator, a reaction thickening separation system and a method, which realize efficient mixing of materials, crystal growth, solution separation and concentration, and automatic cleaning and maintenance of the filtering component by integrating stirring, storage, thickening separation and filtering regeneration systems, thereby improving production efficiency and product quality.

[0005] To achieve the above object, the present invention provides the following technical solutions: The present invention provides a filtering assembly, comprising: a tubular membrane assembly and a liquid collecting pipe assembly; The tubular membrane assembly comprises: a filtration layer and a support layer; One end of the tubular membrane assembly is provided with a threaded joint, and the threaded joint is fixedly connected to the support layer; one end of the threaded joint is connected to the filter layer through a threaded interference fit; a clamp is provided at the periphery of the interference fit connection between the filter layer and the threaded joint, for fixing the filter layer; The liquid collecting pipe assembly comprises: an arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a threaded connection hole and a pipe opening, and the other end of the threaded joint of the tubular membrane module is matched and connected with the threaded connection hole of the arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a tie rod, a first fixing plate and a second fixing plate for fixing the tubular membrane assembly, and the tie rod is provided with a first sleeve and a second sleeve; the first sleeve is fixedly connected to the first fixing plate by a first positioning nut; the second sleeve is fixedly connected to the second fixing plate by a second positioning nut; the length of the tie rod is adjusted by rotating the first positioning nut and the second positioning nut, thereby adjusting the position of the tubular membrane assembly.

[0006] A thickening separator, using the above-mentioned filtering assembly and barrel, and a stirring assembly and a spraying assembly arranged inside the barrel; The stirring assembly is used to make the solution containing the crystals uniform and dispersed to prevent the solution containing the crystals from settling; The filtering assembly is arranged on the inner wall of the cylinder, and is used to separate the clear liquid and the concentrated slurry from the solution containing the crystals, input the clear liquid into the clear liquid tank, and return the concentrated slurry to the reaction kettle, so as to achieve the classification and concentration of the solution; The spray component is used to clean and maintain the filter component in the thickener separator to be regenerated.

[0007] Furthermore, the stirring assembly includes: a motor, a motor bracket, a first agitator, a second agitator, a coupling assembly and a stirring shaft; the output shaft of the motor is connected to the stirring shaft through the coupling assembly, and the stirring shaft and the coupling assembly are fixedly connected by bolts; the first agitator and the second agitator are arranged on the stirring shaft.

[0008] Furthermore, the bottom of the cylinder of the thickening separator is also provided with a liquid inlet, a filtrate outlet, and a thick slurry circulation port; The pipe mouth of the arc-shaped liquid collecting pipe is connected to the filtrate outlet, and the separated clear liquid flows into the clear liquid tank through the pipe mouth of the arc-shaped liquid collecting pipe. A clear liquid regulating valve and a pipeline sight glass are provided on the pipe mouth of each filtrate outlet to observe and control the clear liquid flow rate; The solution containing crystals in the intermediate receiving tank enters the thickening separator through the liquid inlet; the concentrated slurry separated by the thickening separator enters the reactor through the concentrated slurry circulation port; A thick slurry circulation regulating valve is provided at the thick slurry circulation port to adjust the flow rate of the thick slurry returning to the reactor.

[0009] Furthermore, the thickening separator is also provided with a spray port, a forward blowing port, a reverse blowing port, a venting port, a pressure transmitter and a liquid level gauge port; The positive blowing port of the thickening separator is connected to a 0.2Mpa compressed air source through a positive blowing pipeline; The backflush port of the thickening separator is connected to a 0.6Mpa compressed air source through a backflush pipeline; The vent is connected to the intermediate receiving tank through a vent pipe, and is used to adjust the liquid level in the thickener separator through venting; The spray port, forward blowing port, reverse blowing port, venting port, filtrate outlet, liquid inlet and thick slurry circulation port are respectively provided with automatic valves, and each automatic valve is interlockedly controlled by a control system.

[0010] Furthermore, the cylinder is also provided with an ear seat, a manhole and a long sight glass; The ear seat is used to provide a fulcrum for the lifting process during maintenance; The manhole is used for workers to enter the cylinder to perform maintenance, cleaning or inspection of the internal structure; The long sight glass is used for operators to observe the reaction conditions of various materials without opening the cylinder.

[0011] A reaction thickening and separation system, using the above thickening and separation device as well as a reaction kettle, an intermediate receiving tank and a regeneration liquid configuration tank; The reactor is used to fully mix various materials according to certain components and promote the growth of crystals to obtain a solution containing crystals; The intermediate receiving tank is used to store the solution and to provide pressure through a diaphragm pump to transport the solution to the thickening separator; The thickening separator is used to make the solution uniform, dispersed, separated and concentrated, and the solution is separated into a clear liquid and a concentrated slurry through the tubular membrane assembly in the filter assembly of the thickening separator, the clear liquid flows into the clear liquid tank, and the concentrated slurry returns to the reactor; The regeneration liquid configuration tank is used to accurately configure the regeneration liquid using a control system, so as to achieve cleaning and maintenance of the filter components in the thickening separator to be regenerated.

[0012] Furthermore, the control system includes: a PLC controller and a touch screen; The PLC controller is used to obtain the switch signals of the automatic valves at the spray port, backwash port, forward blow port, backwash port, vent port, filtrate outlet, liquid inlet and thick slurry circulation port, and execute the control logic; The touch screen is used to display all operating parameters in the reaction thickening separation system in real time, and allows the staff to manually set the control logic of each automatic valve.

[0013] Furthermore, the operating parameters include: the operating state of the motor, the output flow rate of the clean liquid, the output pressure of the clean liquid, the opening of each valve, the back-blowing pressure, the forward-blowing pressure, the regeneration acid cleaning, and the liquid level.

[0014] A reaction thickening separation method comprises the following steps: (1) Feed preparation; (2) Start stirring: The reactor stirs the feed to form a slurry; (2) Reactor discharge: When the solution in the reactor reaches a certain liquid level, the solution in the reactor automatically overflows from the top of the reactor to the intermediate receiving tank and is pumped into the thickening separator through a diaphragm pump; (3) Separating the solution into a clear liquid and a thick slurry through a filtering component in a thickener separator; (3) The concentrated slurry returns to the reactor through the concentrated slurry circulation port to continue crystal growth, and the clear liquid flows into the clear liquid tank; (4) Backflushing: During the filtration process, backflushing is performed according to the set parameters to remove the solid filter cake on the surface of the tubular membrane assembly; (5) End: When the product is qualified, stop the pump to backwash the pipeline, turn off the filter at the same time, introduce nitrogen to backwash the filter tube, then turn on the forward blow to press all the concentrated slurry back into the reactor and turn off the stirring; (6) Chemical regeneration: Chemical regeneration of the tubular membrane components in the thickener separator is carried out by soaking or filtering the regeneration liquid.

[0015] According to the specific embodiments provided by the present invention, the present invention discloses the following technical effects: The present invention ensures that the materials are fully mixed according to certain components through the reactor, which is beneficial to the uniform progress of the chemical reaction and improves the efficiency and quality of crystal growth. The intermediate receiving tank effectively prevents the solution from settling, ensures the uniformity of the solution, and provides a stable feed liquid for subsequent processing steps; the thickening separator can make the solution uniform, disperse, separate and concentrate, improve the separation efficiency, and effectively separate the clear liquid and the concentrated slurry through the filtering component, thereby maximizing the utilization of resources and reducing operating costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0017] The filter assembly, thickening separator, reaction thickening separation system and method of the present invention are further described below in conjunction with the accompanying drawings; Figure 1 It is a schematic diagram of the overall structure of the reaction thickening and separation system provided by the present invention; Figure 2Schematic diagram of the structure of the thickening separator in the reaction thickening separation system provided by the present invention; wherein (a) is a schematic diagram of a group of tubular membrane components arranged in the reaction thickening separator; (b) is a schematic diagram of two groups of tubular membrane components arranged in the reaction thickening separator and installed upward; (c) is a schematic diagram of two groups of tubular membrane components arranged in the reaction thickening separator and installed downward; Figure 3 It is a schematic diagram of the cross-sectional structure of the arc-shaped liquid collecting pipe in the reaction thickening separation system provided by the present invention; Figure 4 The present invention provides a structural diagram of a tubular membrane assembly in a reaction thickening separation system; wherein (a) is a schematic diagram of a structure in which an intermediate support layer is provided in a filter layer of the tubular membrane assembly; (b) is a schematic diagram of a structure in which an inner support layer is provided in a filter layer of the tubular membrane assembly; (c) is a schematic diagram of a structure in which an outer support layer is provided in a filter layer of the tubular membrane assembly; (d) is a schematic diagram of a structure in which an outer support layer and an inner support layer are provided in a filter layer of the tubular membrane assembly; (e) is a schematic diagram of a structure in which a small gap exists between the inner support layer and the filter layer in a filter layer of the tubular membrane assembly; (f) is a schematic diagram of a structure in which an inner support tube is provided in a filter layer of the tubular membrane assembly and has a small gap between the inner support tube and the filter layer; Figure 5 The present invention provides a schematic diagram of the structure of the arc-shaped liquid collecting pipe in the reaction thickening separation system; (a) is a schematic diagram of the structure of the arc-shaped liquid collecting pipe with a semicircular cross-section; (b) is a schematic diagram of the structure of the arc-shaped liquid collecting pipe with a cross-section smaller than a semicircle; (c) is a quadrilateral with an arc-shaped inner angle; (d) is a quadrilateral with a right-angled inner angle.

[0018] In the figure: 1, reactor; 2, thickening separator; 2-1, motor; 2-2, motor bracket; 2-3, coupling assembly; 2-4, stirring shaft; 2-5, first stirrer; 2-6, second stirrer; 2-7, first positioning nut; 2-8, first sleeve; 2-9, first fixing plate; 2-10, second positioning nut; 2-11, second sleeve; 2-12, second fixing plate; 2-13, pull rod; 2-14, filter element; 2-15, threaded joint; 2-16, arc-shaped liquid collecting pipe; 2-17, support plate; 2-18, reinforcing rib plate; 2-19, thick slurry circulation port; 2-20, liquid inlet; 2-21, filtrate outlet; 2-22, vent; 2-23, pressure transmitter 2-24, liquid level gauge port; 2-25, blowing port; 2-26, spray port; 2-27, manhole; 2-28, ear seat; 2-29, long sight glass; 2-30, first filtrate port; 2-31, second filtrate port; 2-32, third filtrate port; 2-33, fourth filtrate port; 2-34, fifth filtrate port; 2-35, sixth filtrate port; 2-36, seventh filtrate port; 2-37, eighth filtrate port; 2-38, threaded joint; 2-39, gasket; 2-40, clamp; 2-41, filter layer; 2-42, middle support layer; 2-43, inner support layer; 2-44, outer support layer; 2-45, inner support pipe; 3, middle receiving tank; 4, regeneration liquid configuration tank. DETAILED DESCRIPTION

[0019] The specific implementation of the present invention is further described in detail below in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0020] In order to better understand the purpose, structure and function of the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings.

[0021] like Figure 1 As shown, the present invention provides a reaction thickening and separation system, comprising: a reaction kettle 1, an intermediate receiving tank 3, a thickening separator 2, and a regeneration liquid configuration tank 4; The reactor 1 is used to fully mix various materials according to certain components and promote the growth of crystals under chemical reactions to obtain a solution containing crystals; The intermediate receiving tank 3 is used to store the solution to prevent the solution from settling, and to provide pressure through a diaphragm pump to transport the solution to the thickening separator 2; The thickener separator 2 is provided with a first agitator 2-5 and a second agitator 2-6, which are used to uniformly disperse, separate and concentrate the solution, and separate the solution into a clear liquid and a concentrated slurry through a filtering component in the thickener separator 2, the clear liquid flows into a clear liquid tank, and the concentrated slurry returns to the reactor 1.

[0022] The regeneration liquid configuration tank 4 is used to accurately configure the regeneration liquid using a control system to achieve cleaning and maintenance of the filter components in the thickener separator 2 to be regenerated.

[0023] The thickening separator 2 comprises: a cylinder and a stirring assembly, a filtering assembly and a spraying assembly arranged inside the cylinder; The stirring assembly is used to make the solution containing the crystals uniform and dispersed to prevent the solution containing the crystals from settling; The filtering assembly is arranged on the inner wall of the cylinder, and is used to separate the clear liquid and the concentrated slurry from the solution containing the crystals, input the clear liquid into the clear liquid tank, and return the concentrated slurry to the reaction kettle, so as to achieve the classification and concentration of the solution; The spray component is used to clean and maintain the filter component in the thickener separator to be regenerated.

[0024] The stirring assembly includes: a motor 2-1, a motor bracket 2-2, a first agitator 2-5, a second agitator 2-6, a coupling assembly 2-3 and a stirring shaft 2-4; the output shaft of the motor 2-1 is connected to the stirring shaft 2-4 through the coupling assembly 2-3, and the stirring shaft 2-4 is fixedly connected to the coupling assembly 2-3 by bolts; the first agitator 2-5 and the second agitator 2-6 are arranged on the stirring shaft 2-4.

[0025] It should be noted that the stirring assembly adopts a variable frequency motor and a double-layer four-slant-blade open turbine agitator. The stirring shaft is disconnected by a coupling assembly, detachably connected, and fixed with bolts. The stirring blades of the first agitator 2-5 are detachable, the stirring position is adjustable, and a mechanical seal is adopted.

[0026] The filtering component comprises: a tubular membrane component and a liquid collecting pipe component.

[0027] It should be noted that: the arc-shaped liquid collecting pipe is fixed to the support plate 2-17 at the bottom of the cylinder with bolts, and the support plate 2-17 and the reinforcing rib plate 2-18 are welded together with the cylinder; the arc-shaped liquid collecting pipe is a hollow structure, on which are welded several internal threaded joints for installing tubular membrane components, and the cross-section of the arc-shaped liquid collecting pipe can be any semicircular / arc / rectangular structure, and a tie rod for fixing the tubular membrane is welded on the liquid collecting pipe, and a positioning nut / fixing plate and a sleeve are provided on the tie rod, and a 1-layer / 2-layer / 3-layer fixed structure can be set according to the actual design.

[0028] like Figure 2 As shown in (a), the tubular membrane components of the present invention can be arranged in one group, two groups can be arranged to be installed downward, or two groups can be arranged to be installed upward. The installation direction is not unique.

[0029] The filter element 2-14 in the tubular membrane assembly includes: a filtration layer and a support layer.

[0030] A threaded joint 2-15 is provided at one end of the tubular membrane assembly, and the threaded joint 2-15 is fixedly connected to the support layer; one end of the threaded joint 2-15 is connected to the filter layer 2-41 by a threaded interference fit; a clamp 2-40 is provided at the periphery of the interference fit connection between the filter layer 2-41 and the threaded joint 2-15 for fixing the filter layer.

[0031] It should be noted that the support layer in the present invention includes but is not limited to: an inner support layer 2-43, an intermediate support layer 2-42, an outer support layer 2-44 and an inner support tube 2-45. Figure 4 As shown in (a), the filter layer 2-41 is connected to the middle support layer 2-42 by interference fit; Figure 4 As shown in (b), the filter layer 2-41 is connected to the inner support layer 2-43 by interference fit; Figure 4 As shown in (c), the filter layer 2-41 is connected to the external support layer 2-44 by interference fit; Figure 4 As shown in (d), the filter layer 2-41 is respectively connected with the inner support layer 2-43 and the outer support layer 2-44 by interference fit; Figure 4 As shown in (e), an inner support layer 2-43 is provided in the filter layer 2-41, and a small gap exists between the inner support layer 2-43 and the filter layer 2-41; Figure 4 As shown in (f), there is a small gap between the filter layer 2-41 and the inner support tube 2-43; the filter layer is provided with a first filtrate port 2-30, a second filtrate port 2-31, a third filtrate port 2-32, a fourth filtrate port 2-33, a fifth filtrate port 2-34, a sixth filtrate port 2-35, a seventh filtrate port 2-36, and an eighth filtrate port 2-37. In actual applications, the filtrate ports are not unique.

[0032] The tubular membrane module adopts a reinforced tubular membrane. After the support layer in the tubular membrane module is welded and fixed to the left end threaded joint, the filter layer is added through a special process and sintered as a whole, and finally the clamp is installed. Figure 3 As shown, the support layer is a porous plate structure; after the threaded joint 2-15 at the left end of the tubular membrane assembly is welded to the inner support layer, it is fixed to the pre-sintered filter layer through the thread interference fit at the right end of the joint, and then the clamp is installed, wherein there is a small gap between the inner support and the filter layer, wherein the inner support of the tubular membrane assembly is a porous plate structure, and the inner support of the tubular membrane assembly is a steel pipe, and there is a 3-10mm gap between the bottom and the bottom plate of the filter layer.

[0033] The liquid collecting pipe assembly comprises: an arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a threaded connection hole 2-15 and a pipe mouth, and the threaded joint of the tubular membrane module is matched and connected with the threaded connection hole of the arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a tie rod, a first fixing plate 2-9 and a second fixing plate 2-12 for fixing the tubular membrane assembly, and the tie rod is provided with a first sleeve 2-8 and a second sleeve 2-11; the first sleeve 2-8 is fixedly connected to the first fixing plate 2-9 by a first positioning nut 2-7; the second sleeve 2-11 is fixedly connected to the second fixing plate 2-12 by a second positioning nut 2-10; the length of the tie rod is adjusted by rotating the first positioning nut 2-7 and the second positioning nut 2-10, thereby adjusting the position of the tubular membrane assembly.

[0034] The bottom of the cylinder of the thickening separator is also provided with a liquid inlet 2-20, a filtrate outlet 2-21, and a thick slurry circulation port 2-19; The pipe mouth of the arc-shaped liquid collecting pipe is connected to the filtrate outlet 2-21, and the separated clear liquid flows into the clear liquid tank through the pipe mouth of the arc-shaped liquid collecting pipe. A clear liquid regulating valve and a pipeline sight glass are provided on each of the filtrate outlet pipes to observe and control the clear liquid flow rate; The solution containing crystals in the intermediate receiving tank 3 enters the thickening separator 2 through the liquid inlet; the concentrated slurry separated by the thickening separator 2 enters the reactor through the concentrated slurry circulation port; A thick slurry circulation regulating valve is provided at the thick slurry circulation port 2 - 19 for regulating the flow rate of the thick slurry returning to the reaction kettle 1 .

[0035] The thickening separator 2 is also provided with a forward blowing port 2-25, a reverse blowing port, a venting port 2-22, a pressure transmitter 2-23 and a liquid level meter port 2-24; The positive blowing port of the thickening separator is connected to a 0.2Mpa compressed air source through a positive blowing pipeline; The backflush port of the thickening separator is connected to a 0.6Mpa compressed air source through a backflush pipeline; The vent is connected to the intermediate receiving tank through a vent pipe, and is used to adjust the liquid level in the thickener separator by venting; The spray port 2-26, backwash port, forward blowing port 2-25, backwash port, vent port 2-22, filtrate outlet 2-21, liquid inlet 2-20 and thick slurry circulation port 2-19 are respectively provided with automatic valve connections, and each automatic valve is interlockedly controlled through a control system.

[0036] It should be noted that a spray coil is provided on the top of the thickener separator and connected to the spray port. A specific number of nozzles are provided on the spray coil. The spray angle of the nozzle is calculated based on the distance from the nozzle to the tubular membrane and the spray width set by a single nozzle.

[0037] The pipe mouth of the arc-shaped liquid collecting pipe is also provided with one or more of a flow meter, a pressure transmitter or a sampling valve.

[0038] The control system includes: a PLC controller and a touch screen; The PLC controller is used to obtain the switch signals of the automatic valves at the spray port, backwash port, forward blow port, backwash port, vent port, filtrate outlet, feed port and thick slurry circulation port, and execute the control logic; The touch screen is used to display all operating parameters of the reaction thickening separation system in real time, and allows the staff to manually set the control logic of each automatic valve.

[0039] The operating parameters include: the operating state of the motor, the clearing flow rate, the clearing pressure, the valve opening, the back-blowing pressure, the forward-blowing pressure, the regeneration acid cleaning, and the liquid level.

[0040] The cylinder is also provided with ear seats, manholes and long sight glasses; The ear seat 2-28 is used to provide a fulcrum for the lifting process during maintenance; The manhole 2-27 is used for workers to enter the cylinder to perform maintenance, cleaning or inspection of the internal structure; The long sight glass 2-29 is used for the operator to observe the reaction of various materials without opening the cylinder.

[0041] It should be noted that there are three long mirrors 2-29 for observing the situation inside the shell.

[0042] In summary, the reactor of the reaction thickening and separation system of the present invention is provided with a double-layer agitator, a frequency conversion to adjust the speed, and a temperature transmitter / liquid level transmitter / PH detection instrument / pressure transmitter is arranged on the top. Various materials are mixed and reacted in this equipment according to certain components. The reacted solution overflows from the top to the middle receiving tank.

[0043] The middle receiving tank is equipped with a second agitator to prevent material precipitation. A level transmitter and a pressure transmitter are set on the top. The mixed solution enters the thickening separator through the bottom discharge port under the pressure provided by the diaphragm pump. An automatic three-way valve and a thick slurry discharge valve are set at the inlet. A thick slurry circulation regulating valve is set at the bottom of the thickening separator to adjust the flow of the thick slurry back to the reactor at any time. The clear water after passing through the tubular membrane flows out from each collecting pipe. Each collecting pipe is equipped with an automatic valve and a pipeline sight glass. A flow meter / pressure transmitter / sampling valve is set on the clear water outlet main pipe. An automatic valve is set on the reactor pipeline, and a regulating valve is set on the clear liquid tank pipeline to control the clear liquid flow rate.

[0044] A pressure transmitter is installed on the backwash main pipe, and automatic valves are installed at the spray outlet and the backwash outlet respectively, and the signal enters the PLC interlocking control.

[0045] The back-blowing port uses 0.4~0.6Mpa compressed air. A pressure transmitter and automatic valve are installed on the pipeline, and the signal enters the PLC interlocking control.

[0046] The compressed air at the positive blowing port uses 0.2Mpa compressed air. A pressure transmitter and an automatic valve are installed on the pipeline, and the signal enters the PLC interlocking control.

[0047] The regeneration section is equipped with a regeneration tank, with a level meter / overflow pipe / regeneration liquid inlet on the top. A static mixer is set at the regeneration liquid inlet, and a certain amount of 98% sulfuric acid and pure water are respectively introduced for regeneration liquid configuration. Flow meters and regulating valves are set at the inlets of the pure water pipeline and sulfuric acid pipeline to accurately control the concentration of the regeneration liquid configuration. The configured regeneration liquid enters the thickening separator to be regenerated through a pump, and automatic valves are set at the inlet and outlet. Through the PLC program, functions such as automatic solution proportioning / automatic regeneration / automatic reflux can be realized.

[0048] Therefore, the reaction thickening separation system of the present invention is a precision filtration and concentration system suitable for solids ranging from small to large and from small to large. A high-precision tubular membrane is arranged inside the equipment, and a stirring device is arranged on the top to concentrate the solution in the body, and a large amount of concentrated slurry is discharged from the circulation port. A circulation process and a variable frequency stirring process are arranged to achieve uniform mixing and dispersion of materials. The inlet flow rate and the return slurry flow rate are controlled to ensure the stable outflow of the clear liquid and the same liquid output as the inlet flow rate. The liquid level, pressure flow rate are monitored in real time, and the filter is performed when the liquid level is high and the liquid level is closed when the liquid level is too low to ensure that the liquid level of the reactor does not affect the reaction system to continue the crystal growth reaction.

[0049] The process of the present invention is: (a) Synthetic product, the liquid (solution) automatically overflows from the reactor to the intermediate receiving tank; (b) The slurry is pumped from the intermediate receiving tank to the thickening separator through a diaphragm pump; (c) The thickener separator uses pump pressure to discharge the filtered clear liquid from the system through the tubular membrane from the outside to the inside, and the concentrated slurry returns to the reactor through the reflux valve to continue crystal growth to produce qualified products; (d) Compressed gas tank: used for back-blowing regeneration, to periodically back-blow and remove the filter cake layer on the surface of the filter tube; (e) Stirring device: frequency conversion control, stir the solid particles on the surface of the filter tube and in the cylinder evenly, and return them to the reactor in time.

[0050] Requirements for equipment software and control systems (1) According to the process requirements, the mother liquor in the reactor is pumped into the thickening separator. When the liquid level is at the lowest, the stirring is started (without stopping the machine) and the feeding is continued. When the liquid level reaches a high level, the filtrate outlet valve is opened for filtration. After the mother liquor passes through the tubular membrane filtration in the thickening separator, the clear liquid is discharged and the thick slurry returns to the reactor from the bottom for further concentration, forming a closed circulation filtration system.

[0051] (2) Control the feed flow and the return flow of the thick slurry to ensure the stability of the filtrate flow (the flow can be adjusted in real time according to the preset value or curve value); ensure that the amount of filtrate out is the same as the amount of metal salt and liquid alkali in, detect the liquid level, pressure and flow of the liquid level gauge online, filter when the liquid level is high, and shut down when the liquid level is too low to ensure that the liquid level of the reactor does not affect the continued crystal growth of the reaction system. During the filtration process, according to the set interval time or the filtration pressure increase or flow decrease parameters, monitor the liquid level and backflush when it is low to remove the solid filter cake on the surface of the tubular membrane. (3) The whole process is controlled by PLC, one-button start, with a display screen, and self-diagnosis and protection functions. (4) The supply includes a touch screen PLC control cabinet (including touch screen, Siemens host, solenoid valve, contactor, 304 control cabinet, signal line, air pipe, etc.). (5) The thickener separator must have a safe and reliable grounding device to prevent danger caused by leakage; (6) According to the parameters such as the clearing volume, liquid level and pressure in the thickener separator system, the clearing flow rate of the thickener separator is automatically controlled to achieve full automation; (7) The display screen can display all operating parameters of the equipment, including motor operating status, clearing flow, clearing pressure, valve opening, backwash pressure, forward blow pressure, regeneration acid cleaning, liquid level, etc., and can input relevant control parameters; (8) It has a fault alarm function and adopts an audible and visual alarm method. The alarm information includes various alarm functions and various fault displays such as power supply, operation, liquid level, pressure, pressure difference, empty vehicle parking for too long, motor overload shutdown, etc.; (9) It has an emergency stop function. The thickener has an automatic start and stop control function (the thickener separator and the reactor are interlocked: when one fails, it can stop automatically). (10) It can upload operation signals to the DCS in the main control room to ensure that the DCS can be remotely operated. Profibus and Modbus communication protocols are standard, and an Ethernet interface is reserved. The process flow of the present invention is: Feed preparation → Start stirring → Discharge from the top of the reactor → Pump into the bottom of the concentrator with a diaphragm pump → The concentrated slurry returns to the reactor through the electric regulating valve to continue crystal growth → Filter the clear liquid (stable control of the clear liquid flow rate) → Backflush the filter tube during the process → Drain the concentrated slurry → Clean the concentrator → End.

[0052] Feeding: When the reactor slurry reaches a certain liquid level (interlocking can be set), the reactor slurry automatically overflows from the reactor to the intermediate receiving tank; the slurry is pumped from the intermediate receiving tank to the thickening separator through a diaphragm pump; after a certain liquid level, the thickening separator is turned on for stirring; the thickening separator performs slurry filtration and concentration, and the thick slurry is returned to the reactor through a regulating valve to continue to synthesize the spherical balls. The reflux regulating valve is interlocked with the reactor liquid level, and the reactor liquid level fluctuation needs to be controlled within ±0.05m; the initial filtrate contains a small amount of particles that pass through the filtration and returns to the reactor. After the filtrate is clear, it is discharged to the filtrate tank. The filtrate needs to control the flow rate and stabilize the thickening separator liquid level at the same time; 1. Start filtering: After the set time or when the liquid level is set, open the filter liquid outlet valve to start filtering; Filtration: Under the condition of pressure permitting, always check the liquid level of the reactor level gauge and the opening of the regulating valve, control the flow back to the reactor, stabilize the reactor liquid level, and ensure the stability of the flow of the thickener separator filtrate; 2. Backflush: During the filtration process, backflush is performed according to the set parameters such as the intermittent time or the increase in filtration pressure to remove the solid filter cake on the surface of the tubular membrane; 3. End: When the product is qualified, stop the pump to backwash the pipeline, close the filter at the same time, introduce nitrogen to backwash the filter tube, then open the forward blowing to press all the concentrated slurry back to the reactor and turn off the stirring; 4. Use pure water to clean the inside of the equipment (forward wash + backwash), add oil to the reducer, check the sight glass and sealing surface, etc.; 5. Chemical regeneration: The tubular membrane of the thickener separator is chemically regenerated by soaking or filtering in chemical regeneration liquid (10% dilute sulfuric acid).

[0053] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A filter assembly, characterized in that: include: Tubular membrane modules and header modules; The tubular membrane assembly comprises: a filtration layer and a support layer; One end of the tubular membrane assembly is provided with a threaded joint, and the threaded joint is fixedly connected to the support layer; one end of the threaded joint is connected to the filter layer through a threaded interference fit; a clamp is provided at the periphery of the interference fit connection between the filter layer and the threaded joint for fixing the filter layer; The liquid collecting pipe assembly comprises: an arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a threaded connection hole and a pipe opening, and the other end of the threaded joint of the tubular membrane module is matched and connected with the threaded connection hole of the arc-shaped liquid collecting pipe; The arc-shaped liquid collecting pipe is provided with a tie rod, a first fixing plate and a second fixing plate for fixing the tubular membrane assembly, and the tie rod is provided with a first sleeve and a second sleeve; the first sleeve is fixedly connected to the first fixing plate by a first positioning nut; the second sleeve is fixedly connected to the second fixing plate by a second positioning nut; the length of the tie rod is adjusted by rotating the first positioning nut and the second positioning nut, thereby adjusting the position of the tubular membrane assembly.

2. A thickening separator, using the filter assembly according to claim 1, characterized in that: Also includes: A cylinder and a stirring assembly and a spraying assembly arranged inside the cylinder; The stirring assembly is used to make the solution containing the crystals uniform and dispersed to prevent the solution containing the crystals from settling; The filtering assembly is arranged on the inner wall of the cylinder, and is used to separate the clear liquid and the concentrated slurry from the solution containing the crystals, input the clear liquid into the clear liquid tank, and return the concentrated slurry to the reaction kettle, so as to achieve the classification and concentration of the solution; The spray component is used to clean and maintain the filter component in the thickener separator to be regenerated.

3. The thickening separator according to claim 2, characterized in that: The stirring assembly includes: a motor, a motor bracket, a first stirrer, a second stirrer, a coupling assembly and a stirring shaft; the output shaft of the motor is connected to the stirring shaft through the coupling assembly, and the stirring shaft and the coupling assembly are fixedly connected by bolts; the first stirrer and the second stirrer are arranged on the stirring shaft.

4. The thickening separator according to claim 2, characterized in that: The bottom of the cylinder of the thickening separator is also provided with a liquid inlet, a filtrate outlet, and a thick slurry circulation port; The pipe mouth of the arc-shaped liquid collecting pipe is connected to the filtrate outlet, and the separated clear liquid flows into the clear liquid tank through the pipe mouth of the arc-shaped liquid collecting pipe. A clear liquid regulating valve and a pipeline sight glass are provided on the pipe mouth of each filtrate outlet to observe and control the clear liquid flow rate; The solution containing crystals in the intermediate receiving tank enters the thickening separator through the liquid inlet; the concentrated slurry separated by the thickening separator enters the reactor through the concentrated slurry circulation port; A thick slurry circulation regulating valve is provided at the thick slurry circulation port to adjust the flow rate of the thick slurry returning to the reactor.

5. The thickening separator according to claim 2, characterized in that: The thickening separator is also provided with a spray port, a forward blowing port, a reverse blowing port, a venting port, a pressure transmitter and a liquid level gauge port; The positive blowing port of the thickening separator is connected to a 0.2Mpa compressed air source through a positive blowing pipeline; The backflush port of the thickening separator is connected to a 0.6Mpa compressed air source through a backflush pipeline; The vent is connected to the intermediate receiving tank through a vent pipe, and is used to adjust the liquid level in the thickener separator through venting; The spray port, forward blowing port, reverse blowing port, venting port, filtrate outlet, liquid inlet and thick slurry circulation port are respectively provided with automatic valves, and each automatic valve is interlockedly controlled by a control system.

6. The thickening separator according to claim 2, characterized in that: The cylinder is also provided with ear seats, manholes and long sight glasses; The ear seat is used to provide a fulcrum for the lifting process during maintenance; The manhole is used for workers to enter the cylinder to perform maintenance, cleaning or inspection of the internal structure; The long sight glass is used for operators to observe the reaction conditions of various materials without opening the cylinder.

7. A reaction thickening and separation system, using the thickening and separation device according to any one of claims 2 to 6, characterized in that: Also includes: Reactor, intermediate receiving tank, regeneration liquid preparation tank; The reactor is used to fully mix various materials according to certain components and promote the growth of crystals to obtain a solution containing crystals; The intermediate receiving tank is used to store the solution and to provide pressure through a diaphragm pump to transport the solution to the thickening separator; The thickening separator is used to make the solution uniform, dispersed, separated and concentrated, and the solution is separated into a clear liquid and a concentrated slurry through the tubular membrane assembly in the filter assembly of the thickening separator, the clear liquid flows into the clear liquid tank, and the concentrated slurry returns to the reactor; The regeneration liquid configuration tank is used to accurately proportion the regeneration liquid using a control system, so as to achieve cleaning and maintenance of the filter components in the thickening separator to be regenerated.

8. The reaction thickening and separation system according to claim 7, characterized in that: The control system includes: a PLC controller and a touch screen; The PLC controller is used to obtain the switch signals of the automatic valves at the spray port, backwash port, forward blow port, backwash port, vent port, filtrate outlet, liquid inlet and thick slurry circulation port, and execute the control logic; The touch screen is used to display all operating parameters in the reaction thickening separation system in real time, and allows the staff to manually set the control logic of each automatic valve.

9. The reaction thickening and separation system according to claim 8, characterized in that: The operating parameters include: the operating state of the motor, the output flow rate of the clean liquid, the output pressure of the clean liquid, the opening of each valve, the back-blowing pressure, the forward-blowing pressure, the regeneration acid cleaning, and the liquid level.

10. A reaction thickening separation method, using the reaction thickening separation system according to claim 7, characterized in that: The following steps are involved: (1) Feed preparation; (2) Start stirring: The reactor stirs the feed to form a slurry; (2) Reactor discharge: When the solution in the reactor reaches a certain liquid level, the solution in the reactor automatically overflows from the top of the reactor to the intermediate receiving tank and is pumped into the thickening separator through a diaphragm pump; (3) Separating the solution into a clear liquid and a thick slurry through a filtering component in a thickener separator; (3) The concentrated slurry returns to the reactor through the concentrated slurry circulation port to continue crystal growth, and the clear liquid flows into the clear liquid tank; (4) Backflushing: During the filtration process, backflushing is performed according to the set parameters to remove the solid filter cake on the surface of the tubular membrane assembly; (5) End: When the product is qualified, stop the pump to backwash the pipeline, turn off the filter at the same time, introduce nitrogen to backwash the filter tube, then turn on the forward blow to press all the concentrated slurry back into the reactor and turn off the stirring; (6) Chemical regeneration: Chemical regeneration of the tubular membrane components in the thickener separator is carried out by soaking or filtering the regeneration liquid.

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