Ultrafiltration pilot plant and method of use thereof

Abstract

The application provides an ultrafiltration small test device and a use method thereof. The device comprises a tank module and an ultrafiltration module. The tank module comprises a tank body. The bottom of the tank body is provided with a discharge port, and the side of the tank body is provided with a backflow inlet. The tank body is further connected with a cleaning pipeline. The cleaning water inlet of the cleaning pipeline is located outside the tank body, and the water outlet of the cleaning pipeline is located at the top inside the tank body. The ultrafiltration module comprises an ultrafiltration membrane filtration assembly. The ultrafiltration membrane filtration assembly is provided with a liquid inlet and a liquid return port. The discharge port and the liquid inlet of the ultrafiltration membrane filtration assembly are connected with a liquid delivery pipeline. The backflow inlet and the liquid return port of the ultrafiltration membrane filtration assembly are connected with a liquid return pipeline. The permeation port of the ultrafiltration membrane filtration assembly is connected with a permeation pipeline. The end of the permeation pipeline is provided with a first stop valve. The liquid delivery pipeline is provided with an ultrafiltration pump. The liquid return pipeline is connected with a first branch. The end of the first branch is connected with a second stop valve. The first stop valve and the second stop valve can be connected through a first pipeline.

Description

Technical Field

[0001] This application relates to the field of ultrafiltration technology, and more specifically, to an ultrafiltration pilot device and its usage method. Background Technology

[0002] Currently, ultrafiltration equipment is widely used in biopharmaceutical protein purification processes. Users need to conduct small-scale ultrafiltration experiments in the laboratory before large-scale production to identify optimal production processes. However, conventional manual ultrafiltration pilot-scale devices, while small in size, cannot automatically adjust TMP, automatically adjust flow rate, perform online water flux testing of the ultrafiltration membrane, online integrity testing, online equipment cleaning, and online alkali sealing of the ultrafiltration membrane. Furthermore, conventional ultrafiltration equipment can only use one type of ultrafiltration membrane, either a hollow fiber membrane column or a flat sheet membrane pack, which cannot meet the requirements of small-scale testing that requires multiple ultrafiltration membranes. Summary of the Invention

[0003] The purpose of this application is to provide a pilot ultrafiltration device and its usage method to achieve online cleaning of the tank and online alkali sealing of the ultrafiltration membrane.

[0004] The embodiments of this application are implemented as follows:

[0005] In a first aspect, embodiments of this application provide a pilot ultrafiltration device, including a tank module and an ultrafiltration module. The tank module includes a tank body, with a discharge port at the bottom and a return inlet on the side. The tank body is also connected to a cleaning pipeline, with the cleaning water inlet of the cleaning pipeline located outside the tank body and the water outlet of the cleaning pipeline located at the top inside the tank body. The ultrafiltration module includes an ultrafiltration membrane filtration assembly, which has a liquid inlet and a liquid return outlet.

[0006] A liquid delivery pipeline is connected between the outlet and the inlet of the ultrafiltration membrane filter assembly; a return pipeline is connected between the reflux inlet and the return port of the ultrafiltration membrane filter assembly, and the return pipeline is detachably connected to the reflux inlet; a permeate pipeline is connected to the permeate port of the ultrafiltration membrane filter assembly, and a first shut-off valve is installed at the end of the permeate pipeline; an ultrafiltration pump is installed in the liquid delivery pipeline, and the ultrafiltration pump is configured to return the liquid in the tank to the tank after passing through the liquid delivery pipeline, the ultrafiltration membrane filter assembly, and the return pipeline in sequence; a first branch is connected to the return pipeline, and a second shut-off valve is connected at the end of the first branch; the first shut-off valve and the second shut-off valve can be connected through a first pipeline.

[0007] In the ultrafiltration pilot-scale device provided by the above technical solution, since the second shut-off valve at the end of the first branch can be connected to the first shut-off valve at the end of the permeation pipeline through the first pipe, connecting the first shut-off valve and the second shut-off valve through the first pipe allows the liquid in the permeation pipeline to return to the tank via the return pipeline. That is, by connecting the first shut-off valve and the second shut-off valve and adding cleaning water to the tank, the ultrafiltration pump drives the cleaning water to circulate between the first pipe, the tank, and the ultrafiltration membrane filter assembly, achieving online cleaning of the tank and the ultrafiltration membrane filter assembly. Throughout the process, the cleaning water circulates in a closed loop, eliminating the need to add cleaning water midway and reducing waste.

[0008] Furthermore, in the ultrafiltration pilot device provided by the above technical solution, since the outlet of the cleaning pipeline is located at the top of the tank body and the return pipeline is detachably connected to the return inlet, before cleaning the tank body and the ultrafiltration membrane filter assembly, the return pipeline can be connected to the cleaning water inlet of the cleaning pipeline, so that the cleaning water cleans the tank body from the top of the tank body during the circulation process, allowing the tank body to be cleaned more thoroughly.

[0009] In conjunction with the first aspect, in the first embodiment, the return pipeline is further provided with a third shut-off valve, and the first branch is connected between the third shut-off valve and the return inlet; the delivery pipeline is provided with a fourth shut-off valve.

[0010] In the above technical solution, by closing the first, third, and fourth shut-off valves, the pipeline connecting the ultrafiltration membrane filter assembly to the tank or external space can be completely sealed, preventing liquid from flowing out of the ultrafiltration membrane filter assembly. When the liquid sealed in the ultrafiltration membrane filter assembly is alkaline solution, alkaline sealing of the ultrafiltration membrane can be achieved. In the above technical solution, the alkaline solution in the tank can be sent to the delivery pipeline, return pipeline, and permeate side pipeline by the ultrafiltration pump, and then the first, third, and fourth shut-off valves can be closed, thereby achieving online alkaline sealing of the ultrafiltration membrane. Compared with the prior art method of removing the ultrafiltration membrane and soaking it in a container filled with alkaline solution, the alkaline sealing operation in this application is convenient, and there is no need to disassemble or assemble the ultrafiltration membrane before and after alkaline sealing, making the use and alkaline sealing process of the ultrafiltration membrane more efficient.

[0011] In conjunction with the first aspect, in the second embodiment, the fourth shut-off valve is located between the inlet of the ultrafiltration pump and the ultrafiltration membrane filtration assembly; a second branch is connected to the liquid delivery pipeline, which is connected between the ultrafiltration pump and the fourth shut-off valve; a fifth shut-off valve is connected to the end of the second branch, and the fifth shut-off valve and the second shut-off valve can be connected through a second pipeline.

[0012] In the ultrafiltration pilot device provided by the above technical solution, when the fifth shut-off valve and the second shut-off valve are connected through the second pipeline, a loop can be formed between the outlet of the tank and the return inlet, which allows the tank and the remaining pipeline to be cleaned after the ultrafiltration membrane filter module is alkali-sealed online.

[0013] In conjunction with the first aspect, in some embodiments, there are multiple ultrafiltration membrane filter elements, and the liquid supply line, liquid return line and permeation line are used to be detachably connected to one of the multiple ultrafiltration membrane filter elements, and the liquid supply line, liquid return line and permeation line are correspondingly detachably connected to the liquid inlet, liquid return port and permeation port of the same ultrafiltration membrane filter element.

[0014] The ultrafiltration pilot device provided by the above technical solution includes multiple ultrafiltration membrane filtration components. Different ultrafiltration membranes can be used for filtration by connecting different ultrafiltration membrane filtration components to the liquid delivery pipeline, return pipeline and permeation pipeline.

[0015] In conjunction with the first aspect, in some embodiments, the number of ultrafiltration membrane filtration components is two, one being a flat-sheet ultrafiltration membrane and the other being a hollow fiber ultrafiltration membrane column.

[0016] In conjunction with the first aspect, in some embodiments, the bottom of the tank is conical with the tip of the cone pointing downwards, the discharge port is located at the tip of the cone, and the reflux inlet is located on the side of the cone.

[0017] Because the bottom of the tank is conical with the tip pointing downwards, the liquid can reach a certain height when the amount of liquid in the tank is small, thus achieving the function of low-level stirring.

[0018] In conjunction with the first aspect, some embodiments also include a control system connected to the ultrafiltration pump; the delivery pipeline is equipped with a first pressure sensor connected to the control system; the return pipeline is equipped with a first flow meter, a second pressure sensor, and a pressure regulating valve, all connected to the control system; and the through pipeline is equipped with a second flow meter and a third pressure sensor, all connected to the control system.

[0019] In the above technical solution, by connecting the ultrafiltration pump to the control system, the control system can control the ultrafiltration pump to change the flow rate and pressure of the liquid entering the ultrafiltration membrane filtration module. Furthermore, based on the pressure sensors, flow meters, and pressure regulating valves connected to the control system, three ultrafiltration modes—constant flow, constant pressure, and constant TMP—can be automatically achieved through a program.

[0020] Secondly, embodiments of this application provide a method for using an ultrafiltration pilot device to clean the tank in the ultrafiltration pilot device provided in the first aspect. The method includes: disassembling the return liquid pipeline from the return inlet and then connecting it to the cleaning water inlet; connecting the first shut-off valve and the second shut-off valve through a first pipe and opening the first shut-off valve and the second shut-off valve to allow the permeation pipeline to connect to the return liquid pipeline through the first branch; adding cleaning water into the tank and circulating the cleaning water to the tank and the permeation pipeline through an ultrafiltration pump.

[0021] In the above technical solution, by connecting the first and second shut-off valves through a first pipeline, the cleaning water can circulate between the tank, the ultrafiltration membrane filter assembly, the liquid delivery pipeline, the liquid return pipeline, and the permeate pipeline, thereby achieving online cleaning of the tank and the ultrafiltration membrane filter assembly. Compared to the existing technology that requires disassembling each pipeline and rinsing each component, the above method achieves online cleaning of the tank and the ultrafiltration membrane filter assembly without disassembling the pipelines and components, making the operation more convenient and the cleaning efficiency higher.

[0022] Thirdly, embodiments of this application provide a method for using an ultrafiltration pilot device for online alkaline sealing of an ultrafiltration membrane, which is implemented using the ultrafiltration pilot device provided in the second embodiment of the first aspect, and includes a first cleaning step and an alkaline sealing step.

[0023] The first cleaning step includes: disconnecting the return liquid pipeline from the return inlet and then connecting it to the cleaning water inlet; connecting the first shut-off valve and the second shut-off valve through the first pipeline and opening the first shut-off valve and the second shut-off valve to allow the permeable pipeline to connect to the return liquid pipeline through the first branch; adding cleaning water into the tank and circulating the cleaning water to the tank and the permeable pipeline through the ultrafiltration pump.

[0024] The alkali sealing process includes S1: introducing alkali solution into the tank; S2: circulating the alkali solution through an ultrafiltration pump to discharge gas from the ultrafiltration membrane filtration module; and S3: closing the first shut-off valve, the third shut-off valve, and the fourth shut-off valve.

[0025] In the above technical solution, the ultrafiltration membrane is sealed online by connecting the first shut-off valve and the second shut-off valve through the first pipeline, making the operation of sealing the ultrafiltration membrane in the alkaline solution more convenient and efficient.

[0026] In conjunction with the third aspect, in some embodiments, a second cleaning step is included after S3. The second cleaning step includes S4: connecting the second shut-off valve and the fifth shut-off valve through the second pipeline, and introducing cleaning water into the cleaning water inlet to clean the inside of the tank. The cleaning water inside the tank is driven to move outward by the ultrafiltration pump to clean part of the liquid delivery pipeline and part of the liquid return pipeline.

[0027] In the above technical solution, after the ultrafiltration membrane is sealed with alkali online, the remaining pipeline and tank can be connected to form a closed loop by connecting the second and fifth shut-off valves, thereby cleaning the remaining pipeline and tank to remove the alkali solution, making the operation more convenient and efficient. Attached Figure Description

[0028] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this application and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0029] Figure 1 A schematic diagram of the ultrafiltration pilot-scale device provided in the embodiments of this application;

[0030] Figure 2 One of the schematic diagrams for online cleaning using the ultrafiltration pilot-scale device provided in this application;

[0031] Figure 3 Schematic diagram 2 for online cleaning using the ultrafiltration pilot device provided in this application;

[0032] Figure 4 This is a schematic diagram of online alkali sealing of the tank after alkali sealing of the ultrafiltration membrane.

[0033] Icons: 100 - Tank; 110 - Discharge port; 120 - Reflux inlet; 130 - Stirring motor; 140 - Stirring shaft; 200 - Ultrafiltration membrane filter assembly; 210 - Liquid inlet; 220 - Return liquid inlet; 230 - Permeate outlet; 300 - Liquid delivery pipeline; 310 - Ultrafiltration pump; 320 - Fourth shut-off valve; 330 - Fifth shut-off valve; 340 - First pressure sensor; 400 - Return liquid pipeline; 410 - Second shut-off valve; 42 0 - Third shut-off valve; 430 - First flow meter; 440 - Second pressure sensor; 450 - Pressure regulating valve; 460 - Flow tank; 500 - Permeable pipe; 510 - First shut-off valve; 520 - Second flow meter; 530 - Third pressure sensor; 600 - First pipeline; 700 - Cleaning pipeline; 710 - Cleaning water inlet; 720 - Outlet; 730 - Cleaning ball; 800 - Second pipeline; 900 - Make-up pump. Detailed Implementation

[0034] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. The components of the embodiments of this application described and shown in the accompanying drawings can generally be arranged and designed in various different configurations.

[0035] Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely to illustrate selected embodiments of the application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without inventive effort are within the scope of protection of this application.

[0036] It should be noted that similar labels and letters in the following figures indicate similar items. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures.

[0037] In the description of this application, it should be noted that the terms "center," "upper," "lower," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product is in use. They are used only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application. In addition, the terms "first," "second," and "third," etc., are used only to distinguish descriptions and should not be construed as indicating or implying relative importance.

[0038] Furthermore, terms such as "horizontal," "vertical," and "sag" do not imply that components must be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal relative to "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0039] In the description of this application, it should also be noted that, unless otherwise expressly specified and limited, the terms "set up," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.

[0040] The ultrafiltration pilot-scale device is characterized by its simple structure and small size, making it suitable for conducting ultrafiltration pilot-scale tests before large-scale production. The inventors of this application have discovered that existing ultrafiltration pilot-scale devices are inconvenient to clean after use and lack online cleaning capabilities.

[0041] Based on this, the inventors of this application provide an ultrafiltration pilot device and a method for using the ultrafiltration pilot device.

[0042] The ultrafiltration pilot-scale device provided in this application is as follows: Figure 1 As shown, it includes a tank module and an ultrafiltration module. The tank module includes a tank body 100, which is provided with a discharge port 110 and a return inlet 120. The ultrafiltration module includes an ultrafiltration membrane filter assembly 200 containing an ultrafiltration membrane, which has a liquid inlet 210, a liquid return port 220 and a permeation port 230.

[0043] A liquid delivery pipeline 300 is connected between the discharge port 110 and the liquid inlet 210 of the ultrafiltration membrane filter assembly 200; a return pipeline 400 is connected between the reflux inlet 120 and the return port 220 of the ultrafiltration membrane filter assembly 200; a permeation pipeline 500 is connected to the permeation port 230 of the ultrafiltration membrane filter assembly 200, and a first shut-off valve 510 is provided at the end of the permeation pipeline 500. A first branch is connected to the return pipeline 400, and a second shut-off valve 410 is connected at the end of the first branch; the first shut-off valve 510 and the second shut-off valve 410 can be connected through a first pipe 600.

[0044] The liquid delivery pipeline 300 is equipped with an ultrafiltration pump 310. Under the action of the ultrafiltration pump 310, the liquid in the tank 100 can be sent to the ultrafiltration membrane filter assembly 200 for filtration. After the liquid passes through the ultrafiltration membrane filter assembly 200, the large molecules in the liquid return to the tank 100 through the return liquid pipeline 400, and some small molecules enter the permeation pipeline 500.

[0045] The ultrafiltration pilot-scale device provided by the above technical solution can perform ultrafiltration pilot-scale experiments. It should be readily understood by those skilled in the art that during the ultrafiltration experiment, the second shut-off valve 410 should be in the closed state, and the first shut-off valve 510 should be in the open state. Accordingly, this application provides a method for using the above-mentioned ultrafiltration pilot-scale device for cleaning.

[0046] Please combine Figure 1 and Figure 2 The specific usage method includes a first cleaning step, which includes connecting the first shut-off valve 510 and the second shut-off valve 410 via a first pipe 600 (i.e., by...). Figure 1 The provided ultrafiltration pilot device was obtained Figure 2The provided ultrafiltration pilot device is used, and the first shut-off valve 510 and the second shut-off valve 410 are opened, so that the permeate pipe 500 is connected to the return pipe 400 through the first branch. S2: Cleaning water is added to the tank 100, and the ultrafiltration pump 310 is turned on, so that the cleaning water circulates in the tank 100, the liquid delivery pipe 300, the ultrafiltration membrane filter assembly 200, the permeate pipe 500 and the return pipe 400 under the action of the ultrafiltration pump 310, thereby cleaning each pipe and the tank 100. This application does not limit the order of the above operations. Those skilled in the art can perform the above operations in different orders according to the actual situation. For example, cleaning water can be added to the tank 100 first, and then the first shut-off valve 510 and the second shut-off valve 410 can be connected using the first pipe 600; or the first shut-off valve 510 and the second shut-off valve 410 can be connected using the first pipe 600 first, and then cleaning water can be added to the tank 100.

[0047] During the cleaning process using the above method, the cleaning water continuously circulates between the tank 100 and the ultrafiltration membrane filter assembly 200, achieving online cleaning of both. Online cleaning can be understood as cleaning each component while they are connected. Since the first shut-off valve 510 and the second shut-off valve 410 are connected via the first pipe 600, and both valves are open, the cleaning water, after passing through the ultrafiltration membrane, sequentially passes through the permeate pipe 500 and the return pipe 400 before returning to the tank 100. Therefore, there is no loss of cleaning water during the cleaning process, and there is no need to continuously add cleaning water. Those skilled in the art can select the cleaning water according to actual needs; for example, purified water, alkaline solution, or sodium chloride solution can be selected.

[0048] In practical applications, the feed solution used in ultrafiltration pilot experiments is often a protein solution. When the protein solution enters the tank 100 through the return pipe 400, if the feed solution leaves from the top of the tank 100, foam will be generated as the feed solution falls and impacts the liquid surface inside the tank 100. Therefore, in a preferred embodiment of the ultrafiltration pilot device provided in this application, the return inlet 120 is located on the side of the tank 100. That is, when the feed solution enters the tank 100 through the return inlet 120, the feed solution can leave along the side wall of the tank 100, thus avoiding the generation of foam.

[0049] In the above embodiments, the reflux inlet 120 is located on the side of the tank 100. During the cleaning of the ultrafiltration pilot device using the method provided in this application, the cleaning water flows from the side wall of the tank 100 into the tank 100 and then falls to the bottom of the tank 100, making it difficult to clean the top of the tank 100. Therefore, in a preferred embodiment of this application, the tank 100 is also connected to a cleaning pipeline 700. The cleaning water inlet 710 of the cleaning pipeline 700 is located on the outside of the tank 100, and the outlet 720 of the cleaning pipeline 700 is located at the top inside the tank 100. Furthermore, the return pipeline 400 is detachably connected to the reflux inlet 120 of the tank 100. After the return pipeline 400 is detached from the reflux inlet 120 of the tank 100, it can be connected to the cleaning water inlet 710 of the cleaning pipeline 700. Preferably, a cleaning ball 730 is also connected at the water outlet 720. The cleaning ball 730 is a spherical structure with multiple through holes on its surface. When the cleaning water flows out from the cleaning ball 730, it can be sprayed into different positions inside the tank 100 through the through holes at different positions.

[0050] Accordingly, the method for cleaning the ultrafiltration pilot device provided in the above embodiment includes disconnecting the return liquid pipeline 400 from the return inlet 120 and then connecting it to the cleaning water inlet 710 (i.e., the connection position between the tank 100 and the return liquid pipeline 400 is from...). Figure 1 Switch to as shown Figure 3 (As shown); connect the first shut-off valve 510 and the second shut-off valve 410 through the first pipe 600, and open the first shut-off valve 510 and the second shut-off valve 410, so that the permeate pipe 500 is connected to the return pipe 400 through the first branch; add cleaning water into the tank 100, and use the ultrafiltration pump 310 to circulate and clean the tank 100, the delivery pipe 300, the ultrafiltration membrane filter assembly 200, the return pipe 400, and the permeate pipe 500. The process of disconnecting the return pipe 400 from the return inlet 120 and connecting it to the cleaning water inlet 710 does not affect the connection between the return pipe 400 and the return port 220 of the ultrafiltration membrane filter assembly 200. This application does not limit the order of the above operations. Those skilled in the art can perform the above operations in different orders according to the actual situation. For example, the first shut-off valve 510 and the second shut-off valve 410 can be connected first using the first pipe 600, and then the return pipe 400 can be connected to the cleaning water inlet 710; or the return pipe 400 can be connected to the cleaning water inlet 710 first, and then the first shut-off valve 510 and the second shut-off valve 410 can be connected using the first pipe 600.

[0051] Due to further optimization of the structure of the ultrafiltration pilot device, in the above-described method of use, the return liquid line 400 is adapted to be switched from being connected to the return inlet 120 to being connected to the cleaning water inlet 710, so that the ultrafiltration pilot device can be used in accordance with... Figure 3 During the online cleaning process shown, cleaning water flows out from the top inside the tank 100, which can clean the top of the tank 100 to a certain extent.

[0052] In the above embodiments, there are no special restrictions on the form of the cleaning pipeline 700, as long as the cleaning pipeline 700 can enable the cleaning water to flow out from the top of the tank 100. For example, in some embodiments, the cleaning pipeline 700 can be a connector connected to the top of the tank 100 and capable of docking with the return pipeline 400.

[0053] In some embodiments of the ultrafiltration pilot-scale device provided in this application, in order to achieve online alkali sealing of the ultrafiltration membrane, such as... Figures 1 to 3 As shown, the return pipeline 400 is also equipped with a third shut-off valve 420, and a first branch connects the third shut-off valve 420 and the return inlet 120; a fourth shut-off valve 320 is installed on the delivery pipeline 300. The connection between the first branch and the third shut-off valve 420 and the return inlet 120 should be understood as follows: in the flow path of the liquid in the return pipeline 400, the liquid first passes through the third shut-off valve 420, then through the location where the first branch connects to the return pipeline 400, and finally reaches the return inlet 120 on the tank 100. Those skilled in the art will readily understand that the third shut-off valve 420 should be in the open state during ultrafiltration experiments.

[0054] Accordingly, this application also provides a method for using the ultrafiltration pilot device provided in the above embodiments to perform online alkaline sealing of the ultrafiltration membrane, including an alkaline sealing step. Those skilled in the art can perform online cleaning using the first cleaning step in the cleaning method provided in the above embodiments before alkaline sealing, and then perform online alkaline sealing of the ultrafiltration membrane with the pipeline connection at the time of the first cleaning step completion. The alkaline sealing step includes: S1: Introducing alkaline solution into the tank 100, and connecting the first shut-off valve 510 and the second shut-off valve 410 through the first pipeline 600 (i.e., Figure 2 or Figure 3(As shown), and open the first shut-off valve 510 and the second shut-off valve 410, so that the permeate pipe 500 is connected to the return pipe 400 through the first branch; S2: The alkali solution is circulated by the ultrafiltration pump 310 to discharge the gas in the ultrafiltration membrane filter assembly 200; S3: The first shut-off valve 510, the third shut-off valve 420 and the fourth shut-off valve 320 are closed. In the above step S2, the ultrafiltration pump 310 fills the delivery pipe 300 and the return pipe 400 with alkali solution. Since the alkali solution contains small molecules that can pass through the ultrafiltration membrane, the alkali solution will also fill the permeate pipe 500 after passing through the ultrafiltration membrane. After closing the first shut-off valve 510, the third shut-off valve 420 and the fourth shut-off valve 320, the permeate pipe 500, the return pipe 400 and the delivery pipe 300 can be cut off respectively. The alkaline solution located on one side of the ultrafiltration membrane filter assembly 200 through the pipeline 500, the return liquid pipeline 400 and the delivery liquid pipeline 300 cannot flow, thereby sealing the ultrafiltration membrane in the alkaline environment and realizing online alkaline sealing of the ultrafiltration membrane.

[0055] Furthermore, in some embodiments of the ultrafiltration pilot device, the fourth shut-off valve 320 is located between the ultrafiltration pump 310 and the inlet 210 of the ultrafiltration membrane filtration assembly 200; a second branch is connected above it, and the second branch connects between the ultrafiltration pump 310 and the fourth shut-off valve 320. For example... Figures 1 to 4 As shown, the second branch is connected to a fifth shut-off valve 330 at its end, as... Figure 4 As shown, the fifth shut-off valve 330 is a valve used for discharging material. It can be used to discharge the liquid in the liquid delivery pipeline 300 after the ultrafiltration production is completed. The fifth shut-off valve 330 and the second shut-off valve 410 can be connected through the second pipeline 800.

[0056] After completing the online alkali sealing of the ultrafiltration membrane, the ultrafiltration pilot device provided by the above technical solution can clean the tank 100 and the pipelines containing residual alkali in the liquid delivery pipeline 300 and the return pipeline 400. The specific cleaning method includes a second cleaning step, which includes a step S4 following step S3 above. S4 includes connecting the second shut-off valve 410 and the fifth shut-off valve 330 through the second pipeline 800, and introducing cleaning water into the cleaning water inlet 710 to clean the inside of the tank 100. The cleaning water in the tank 100 is driven to move outward by the ultrafiltration pump 310 to clean part of the liquid delivery pipeline 300 and part of the return pipeline 400. Of course, to achieve a more comprehensive cleaning of the tank 100, before starting the ultrafiltration pump 310 to clean the tank 100, the return pipe 400 can be switched from being connected to the return inlet 120 of the tank 100 to being connected to the cleaning water inlet 710. This allows the cleaning water to flow down from the top inside the tank 100 during circulation, resulting in a more thorough cleaning of the tank 100. Those skilled in the art will readily understand that after online alkali sealing of the ultrafiltration membrane, the third shut-off valve 420 and the fourth shut-off valve 320 are closed. Therefore, after connecting the delivery pipe 300 and the return pipe 400 through the second pipe 800, the cleaning water, under the action of the ultrafiltration pump 310, enters the delivery pipe 300 from the tank, then enters the return pipe 400 through the second pipe 800, and finally returns to the tank 100. This achieves online cleaning of the tank 100 and the pipes in the delivery pipe 300 and return pipe 400 that contain residual alkali.

[0057] The ultrafiltration pilot device provided in the above embodiments can perform online cleaning of the tank 100 after online alkaline sealing of the ultrafiltration membrane, which is convenient and easy to operate.

[0058] In some embodiments of this application, the tank 100 is also connected to a replenishment pump 900, which is used to deliver liquids such as buffer solution, cleaning water or alkaline solution into the tank 100 to replenish the liquid during the ultrafiltration process or to clean the tank 100.

[0059] In some embodiments of the ultrafiltration pilot-scale apparatus provided in this application, the ultrafiltration module includes multiple ultrafiltration membrane filter components 200. During each ultrafiltration experiment, the liquid delivery line 300, the liquid return line 400, and the permeation line 500 are all connected to the same ultrafiltration membrane filter component 200. "Multiple" refers to two or more. Furthermore, the ultrafiltration membranes in different ultrafiltration membrane filter components 200 are of different types, so that operators can select different ultrafiltration membranes for experiments when using the ultrafiltration pilot-scale apparatus provided in this application. For example, the ultrafiltration membrane in one ultrafiltration membrane filter component 200 is a flat-sheet ultrafiltration membrane, and the ultrafiltration membrane in another ultrafiltration membrane filter component 200 is a hollow fiber ultrafiltration membrane column.

[0060] In some embodiments of this application, a stirring shaft 140 is also provided inside the tank 100. The stirring shaft 140 can stir the liquid to be used in the ultrafiltration experiment; it can also stir the cleaning water to make the cleaning of the tank 100 more thorough. Furthermore, the bottom of the tank 100 is conical, with the tip of the cone pointing downwards. Therefore, when the liquid volume in the tank 100 is small, the liquid can form a certain height, achieving the function of low-level stirring. The bottom of the tank 100 can be conical.

[0061] Furthermore, the discharge port 110 is located at the tip of the cone, and the reflux inlet 120 is located on the side of the cone-shaped portion of the tank 100, so that when the liquid enters the tank 100 from the reflux inlet 120, the liquid can flow along the slope towards the bottom of the tank 100, thereby reducing the foam generated when the liquid entering the tank 100 is a protein solution.

[0062] In some embodiments, a stirring motor 130 is connected to the upper end of the tank 100, and a vertically arranged stirring shaft 140 is provided in the cavity, with the stirring shaft 140 being drivenly connected to the output shaft of the stirring motor 130.

[0063] In some implementations of ultrafiltration pilot-scale devices, to make the ultrafiltration experimental process more controllable, a control system connected to the ultrafiltration pump 310 is also included. The liquid delivery line 300 is equipped with a first pressure sensor 340 connected to the control system; the return line 400 is equipped with a first flow meter 430, a second pressure sensor 440, and a pressure regulating valve 450, all connected to the control system; and the permeation line 500 is equipped with a second flow meter 520 and a third pressure sensor 530, both connected to the control system. Furthermore, a flow cell 460 is also provided on the return line 400, and the second pressure sensor 440 is installed in the flow cell 460. Conductivity meters, pH meters, and other measuring instruments can also be installed on the flow cell 460.

[0064] In the above technical solution, the control system can control the rotation speed of the ultrafiltration pump 310, thereby adjusting the inlet flow rate and inlet pressure, thus enabling both constant flow and constant pressure ultrafiltration modes. The TMP value can be calculated using the values ​​measured by the first pressure sensor 340, the second pressure sensor 440, and the third pressure sensor 530 in the above technical solution. The TMP value can be changed by adjusting the pressure regulating valve 450 through the control system, thus enabling a constant TMP filtration mode. Furthermore, the control system can also control the rotation speed of the replenishment pump 900 based on the data measured by the second flow meter 520, achieving equal-volume washing filtration. That is, the amount of liquid permeating through the ultrafiltration membrane is matched by the amount of liquid delivered to the tank 100 by the replenishment pump 900, maintaining a constant liquid volume within the equipment. The second flow meter 520 in the above technical solution can also be used for online water flux testing of the ultrafiltration membrane. The first shut-off valve 510, the second shut-off valve 410, and the fifth shut-off valve 330 in this application also provide operators with interfaces to connect the ultrafiltration pilot device to other components. For example, the second shut-off valve 410 can be connected to an integrity tester to achieve online integrity testing of the ultrafiltration membrane.

[0065] In this application, the ultrafiltration pump 310 and the replenishment pump 900 can be low-shear transfer pumps in the prior art, such as quaternary diaphragm pumps, peristaltic pumps, rotary pumps, etc., to prevent protein breakage due to shearing. Those skilled in the art can select from existing sanitary low-shear transfer pumps according to actual usage needs.

[0066] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. An ultrafiltration pilot plant device, characterized in that, The application relates to a small-scale ultrafiltration device, which comprises a tank module and an ultrafiltration module. The tank module comprises a tank body, the bottom of the tank body is provided with a discharge port, the side of the tank body is provided with a backflow inlet, and a cleaning pipeline is connected to the tank body. The cleaning water inlet of the cleaning pipeline is located outside the tank body, and the water outlet of the cleaning pipeline is located at the top of the tank body. The ultrafiltration module comprises an ultrafiltration membrane filtration assembly which has a liquid inlet and a liquid return port. A liquid feeding pipeline is connected between the discharge port and the liquid inlet of the ultrafiltration membrane filtration assembly. A liquid return pipeline is connected between the backflow inlet and the liquid return port of the ultrafiltration membrane filtration assembly. The liquid return pipeline is detachably connected to the backflow inlet.

2. The ultrafiltration pilot plant device according to claim 1, characterized in that The permeation port of the ultrafiltration membrane filtration assembly is connected with a permeation pipeline, and the end of the permeation pipeline is provided with a first stop valve.

3. The ultrafiltration pilot plant device according to claim 2, characterized in that The liquid feeding pipeline is provided with an ultrafiltration pump.

4. The ultrafiltration pilot plant device according to claim 1, characterized in that The ultrafiltration pump is configured to make the liquid in the tank body pass through the liquid feeding pipeline, the ultrafiltration membrane filtration assembly and the liquid return pipeline in sequence and then return to the tank body.

5. The ultrafiltration pilot plant device according to claim 1, characterized in that The liquid return pipeline is connected with a first branch, and the end of the first branch is connected with a second stop valve.

6. A method of using an ultrafiltration pilot plant, characterized by When the ultrafiltration membrane is subjected to online alkali sealing, the first stop valve and the second stop valve are connected through a first pipeline. The liquid return pipeline is further provided with a third stop valve. The first branch is connected between the third stop valve and the backflow inlet. The fourth stop valve is located between the ultrafiltration pump and the liquid inlet of the ultrafiltration membrane filtration assembly. The liquid feeding pipeline is connected with a second branch. The end of the second branch is connected with a fifth stop valve. After the ultrafiltration membrane is subjected to online alkali sealing, the first pipeline connected between the first stop valve and the second stop valve is removed, and the fifth stop valve and the second stop valve are connected through a second pipeline. The number of the ultrafiltration membrane filtration assemblies is plural. The liquid feeding pipeline, the liquid return pipeline and the permeation pipeline are used for detachable connection with one of the plural ultrafiltration membrane filtration assemblies. The number of the ultrafiltration membrane filtration assemblies is two, one of which is a flat plate type ultrafiltration membrane, and the other is a hollow fiber ultrafiltration membrane column. The bottom of the tank body is conical, the tip of the cone faces downward, the discharge port is located at the tip of the cone, and the backflow inlet is located on the side of the cone. The control system is signal-connected with the ultrafiltration pump. The liquid feeding pipeline is provided with a first pressure sensor which is signal-connected with the control system. The liquid return pipeline is provided with a first flow meter, a second pressure sensor and a pressure regulating valve which are all signal-connected with the control system. The tank body and the permeation pipeline in the small-scale ultrafiltration device are cleaned. The return liquid pipeline is detached from the return inlet, and then connected with the cleaning water inlet; the first stop valve and the second stop valve are connected through a first pipeline, and the first stop valve and the second stop valve are opened, so that the permeation pipeline is communicated with the return liquid pipeline through the first branch; Cleaning water is added into the tank, and the cleaning water is circulated to clean the tank and the permeation pipeline through an ultrafiltration pump.

7. A method of using an ultrafiltration pilot plant, characterized by The ultrafiltration small test device of claim 1 is used to realize online alkali sealing of an ultrafiltration membrane, and includes a first cleaning step and an alkali sealing step; The first cleaning step includes: The return liquid pipeline is detached from the return inlet, and then connected with the cleaning water inlet; the first stop valve and the second stop valve are connected through a first pipeline, and the first stop valve and the second stop valve are opened, so that the permeation pipeline is communicated with the return liquid pipeline through the first branch; cleaning water is added into the tank, and the cleaning water is circulated to clean the tank and the permeation pipeline through an ultrafiltration pump. The alkali sealing step includes: S1: the cleaning water in the first cleaning step is discharged, and alkali solution is introduced into the tank; S2: the alkali solution is circulated through the ultrafiltration pump to discharge gas in the ultrafiltration membrane filtration assembly; S3: the first stop valve, the third stop valve and the fourth stop valve are closed.

8. The method of use of claim 7, wherein, After S3, a second cleaning step is further included, and the second cleaning step includes S4: the second stop valve and the fifth stop valve are communicated through a second pipeline, cleaning water is introduced into the cleaning water inlet to clean the inside of the tank, and the cleaning water in the tank is driven to move outward through the ultrafiltration pump to clean part of the liquid feeding pipeline and part of the return liquid pipeline.

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