Multistage countercurrent water inlet type mixed bed resin complete separation method and device for laboratory

Abstract

The invention discloses a multi-stage countercurrent water inlet type mixed bed resin complete separation method and device for a laboratory, and belongs to the technical field of mixed bed ion exchange resin separation. According to the device disclosed by the invention, the multi-stage resin separation column system, the anion resin collection system and the control system are arranged, the mixed bed ion exchange resin in the resin separation columns is in a fluidized state by controlling the ascending flow of the demineralized water, the resin is continuously scrubbed by utilizing the demineralized water, surface pollutants are removed, and the separation efficiency is improved. And the anion exchange resin and the cation exchange resin are completely separated after passing through a multi-stage resin separation column system through forced countercurrent backwashing, so that the technical problem that the separation of the anion exchange resin and the cation exchange resin is difficult to realize by the existing method is solved.

Description

Technical Field

[0001] The invention belongs to the technical field of mixed bed ion exchange resin separation, and in particular relates to a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method and device. Background Art

[0002] As an efficient and multifunctional separation material, ion exchange resin plays a vital role in many industries. Its unique ion exchange capacity makes it show a wide range of application potential in many fields. In the field of water treatment, the importance of ion exchange resin is particularly prominent. As one of the important means of water purification, it can not only effectively remove impurities and harmful substances in water, but also adjust the pH and hardness of water to ensure the safety and stability of water quality. In the complex water treatment process of power plants, ion exchange resin is an indispensable key link. It can help power plants remove ionic pollutants in water, prevent equipment corrosion and scaling, and improve the operating efficiency and stability of the system. In addition, ion exchange resin also plays an important role in the food industry and the pharmaceutical industry. In the food industry, it can be used for decolorization, impurity removal and purification of food to improve the quality and safety of food. In the pharmaceutical industry, ion exchange resin is widely used in the separation, purification and preparation of drugs, providing strong support for the production of drugs.

[0003] According to the different charge properties, ion exchange resins are mainly divided into two categories: anion exchange resins and cation exchange resins. These two resins can be used alone or mixed in different proportions according to specific needs to construct an ion exchange cation bed system, an ion exchange anion bed system or a more efficient ion exchange mixed bed system. These systems have their own characteristics and can meet the requirements of different water quality treatments and achieve accurate removal and balance of ions in water. It is particularly worth mentioning that the ion exchange mixed bed system is often used as a deep treatment method after pretreatment processes such as reverse osmosis to produce high-quality demineralized water due to its excellent ion removal ability and water quality improvement effect. After the reverse osmosis technology effectively removes most of the soluble solids, the mixed bed system can further remove the residual trace ions, including silicate ions that are difficult to remove, thereby ensuring that the effluent water quality reaches extremely high purity and meets the stringent requirements of high water use standards industries such as power generation and chemical industry.

[0004] However, with the continuous operation of the mixed bed ion exchange resin, the physical and chemical properties of the resin need to be monitored regularly. The resin layer in the mixed bed is composed of anion exchange resin and cation exchange resin. After sampling, it is usually necessary to completely separate the anion exchange resin and the cation exchange resin and then test their physical and chemical properties according to the corresponding methods to determine whether they can continue to be used. As we all know, the density of anion exchange resin and cation exchange resin is similar, and the density of anion exchange resin is slightly smaller than that of cation exchange resin, which makes it difficult to separate them quickly, causing great difficulties for the subsequent accurate detection of their physical and chemical properties. Summary of the invention

[0005] The object of the present invention is to provide a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method and device, which is used to solve the technical problem that the existing method is difficult to achieve the separation of anion exchange resin and cation exchange resin.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions: The invention discloses a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device, comprising a desalted water tank, a circulation pump, a multi-stage resin separation column system, an anion resin collection system and a control system; One end of the desalted water tank, the circulation pump, the multi-stage resin separation column system and one end of the anion resin collection system are connected in sequence, and the other end of the desalted water tank and the other end of the anion resin collector are connected to form a circulation loop; The circulation pump and the anion resin collection system are respectively connected to the control system.

[0007] Further, the multi-stage resin separation column system comprises a first-stage resin separation column, a second-stage resin separation column and a third-stage resin separation column connected in sequence; The first-stage resin separation column is connected to a circulation pump; the third-stage resin separation column is connected to an anion resin collection system.

[0008] Furthermore, the anion resin collection system includes a sand core filter plate, a quality sensor, a liquid level sensor and an anion resin collector; the two ends of the anion resin collector are respectively connected to the third-stage resin separation column and the desalted water tank; the sand core filter plate is arranged inside the anion resin collector; the quality sensor and the liquid level sensor are both arranged below the sand core filter plate.

[0009] Furthermore, the control system includes a controller and a computer connected to each other; the mass sensor and the liquid level sensor are both connected to the controller.

[0010] Furthermore, a solenoid valve is also provided on the pipeline connecting the desalted water tank and the anion resin collector.

[0011] Furthermore, the solenoid valve is connected to a controller.

[0012] The present invention also discloses a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method, which is implemented by using the above-mentioned device and includes the following steps: First, desalted water is added to the desalted water tank, and then mixed bed resin is added to the multi-stage resin separation column system; The control system sends instructions to the circulation pump to continuously feed the desalted water into the multi-stage resin separation column system, so that the mixed bed resin enters a fluidized state; then the control system controls the circulation pump so that the multi-stage resin separation column system obtains the desalted water mixed with the ion exchange resin, and enters the anion resin collection system to obtain the anion exchange resin and desalted water.

[0013] Further, the anion resin collection system includes an anion resin collector; The control system includes a controller and a computer connected to each other; When performing separation, the following steps are specifically included: The computer sends instructions to the controller, and the controller sends instructions to the circulation pump, which starts to rotate, so that the desalted water continuously enters the first-stage resin separation column. At this time, the mixed bed ion exchange resin in the mixed bed resin gradually enters the fluidized state; Wait for the mixed bed ion exchange resin in the mixed bed resin to be completely dispersed, and adjust the speed of the circulation pump until the desalted water in the first-stage resin separation column is filled, and then the desalted water mixed with the ion exchange resin overflows into the second-stage resin separation column; as the desalted water mixed with the ion exchange resin in the second-stage resin separation column is filled, the desalted water mixed with the ion exchange resin overflows into the third-stage resin separation column; as the third-stage resin separation column is filled, the desalted water mixed with the ion exchange resin finally overflows into the anion exchange resin collector.

[0014] Furthermore, the anion resin collection system also includes a sand core filter plate, a quality sensor, and a liquid level sensor; a solenoid valve is also provided on the pipeline connecting the desalted water tank and the anion resin collector; when performing separation, the following steps are specifically included: The deionized water mixed with ion exchange resin flowing into the anion exchange resin collector is separated into anion exchange resin and deionized water by the sand core filter plate; when the level of the anion exchange resin or deionized water on the sand core filter plate reaches the standard, it is fed back to the controller and then to the computer; The computer sends a command to the controller, the circulation pump stops rotating, and the solenoid valve at the bottom of the anion exchange resin collector opens, and the desalted water circulates into the desalted water tank; The anion exchange resin is taken out from the upper part of the anion resin collector, and the cation exchange resin is taken out from the lower part of the first-stage resin separation column.

[0015] Furthermore, the level of the anion exchange resin or deionized water in the upper part of the sand core filter plate reaches the standard that the mass of the anion exchange resin is greater than 100 g or the level of the deionized water reaches 15 cm.

[0016] Compared with the prior art, the present invention has the following beneficial effects: The invention discloses a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device. By arranging a multi-stage resin separation column system, an anion resin collection system and a control system, the mixed bed ion exchange resin in the resin separation column is in a fluidized state by controlling the rising flow rate of desalted water, the resin is continuously scrubbed with desalted water to remove surface pollutants, and the anion exchange resin and the cation exchange resin are completely separated after passing through the multi-stage resin separation column system by forced countercurrent backwashing, thereby solving the technical problem that the existing method is difficult to separate the anion exchange resin and the cation exchange resin.

[0017] The multi-stage resin separation column system is designed to be composed of three-stage separation columns in series, and the three-stage separation columns are connected in sequence through polytetrafluoroethylene pipes. The heights of the three-stage separation columns are reduced in sequence. By controlling the rising flow rate of desalted water, the mixed bed ion exchange resin in the resin separation column is in a fluidized state. The resin is continuously scrubbed with desalted water to remove surface pollutants, and the anion and cation exchange resins are completely separated after passing through the three-stage separation column through forced countercurrent backwashing. The cation exchange resin is deposited at the bottom of the first-stage separation column due to its large density, while the anion exchange resin has a small density and is collected in the anion resin collector after the three-stage separation column. This method has high separation efficiency, simple control method, and broad application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the structure of a multi-stage countercurrent water inflow mixed bed resin complete separation device for laboratory use of the present invention; Figure 2 A schematic diagram of a mixed bed ion exchange resin to be separated using the present invention; Figure 3 A schematic diagram of an anion exchange resin obtained by separation using the device of the present invention; Figure 4 A schematic diagram of a cation exchange resin obtained by separation using the device of the present invention; Among them: 1-first stage resin separation column; 2-second stage resin separation column; 3-third stage resin separation column; 4-circulation pump; 5-deionized water tank; 6-controller; 7-computer; 8-sand core filter plate; 9-weight sensor; 10-liquid level sensor; 11-solenoid valve; 12-anion exchange resin collector. DETAILED DESCRIPTION

[0019] In order to enable those skilled in the art to understand the characteristics and effects of the present invention, the following is a general description and definition of the terms and expressions mentioned in the specification and claims. Unless otherwise specified, all technical and scientific terms used in the text are the common meanings understood by those skilled in the art for the present invention. In the event of a conflict, the definition in this specification shall prevail.

[0020] The theories or mechanisms described and disclosed herein, whether correct or incorrect, should not limit the scope of the present invention in any way, that is, the present invention can be implemented without being limited by any specific theory or mechanism.

[0021] In this article, all features such as values, quantities, contents and concentrations defined in the form of numerical ranges or percentage ranges are for simplicity and convenience only. Accordingly, the description of numerical ranges or percentage ranges should be considered to have included and specifically disclosed all possible secondary ranges and individual values ​​within the range (including integers and fractions).

[0022] In this document, unless otherwise specified, “includes,” “including,” “contains,” “has,” or similar terms cover the meanings of “consisting of” and “mainly consisting of,” for example, “A includes a” covers the meanings of “A includes a and other” and “A only includes a.”

[0023] In this document, in order to make the description concise, not all possible combinations of various technical features in various embodiments or examples are described. Therefore, as long as there is no contradiction in the combination of these technical features, the various technical features in various embodiments or examples can be combined arbitrarily, and all possible combinations should be considered to be within the scope of this specification.

[0024] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0025] The following examples use conventional instruments and equipment in the art. The experimental methods in the following examples where specific conditions are not specified are usually carried out under conventional conditions or under conditions recommended by the manufacturer. The various raw materials used in the following examples are conventional commercial products unless otherwise specified, and their specifications are conventional specifications in the art. In the specification of the present invention and the following examples, unless otherwise specified, "%" means weight percentage, "part" means weight part, and ratio means weight ratio.

[0026] The present invention is further described in detail below in conjunction with the accompanying drawings: See also Figure 1 As shown, the present invention discloses a laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device, comprising a desalted water tank 5, a circulating pump 4, a multi-stage resin separation column system, an anion resin collection system and a control system; wherein the multi-stage resin separation column system comprises a first-stage resin separation column 1, a second-stage resin separation column 2 and a third-stage resin separation column 3 connected in sequence; and the first-stage resin separation column 1, the second-stage resin separation column 2 and the third-stage resin separation column 3 are connected in sequence through a polytetrafluoroethylene pipeline, and the height of the three-stage separation column decreases in sequence.

[0027] Among them, the anion resin collection system includes a sand core filter plate 8, a mass sensor 9, a liquid level sensor 10 and an anion resin collector 12; the control system includes a controller 6 and a computer 7 that are connected to each other; the circulation pump 4, the liquid level sensor 10, the solenoid valve 11, the weight sensor 9, etc. are connected to the controller 6 through a data communication line, and the computer 7 issues instructions to the controller 6; the bottom of the anion resin collector 12 is connected to the deionized water tank 5 through a polytetrafluoroethylene pipeline to form a circulation loop; the anion exchange resin collector 12 has a sand core filter plate 8 in the middle to separate the deionized water and the anion exchange resin coming out of the resin separation column, and at the same time, a weight sensor 9 is provided under the sand core filter plate 8 to measure the mass of the anion exchange resin; the middle of the anion resin exchanger 12 has a liquid level sensor 10 to monitor the liquid level height therein.

[0028] When the above-mentioned laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device is used for separation, the following steps are included: Step 1: Fill the desalted water tank 5 with desalted water.

[0029] Step 2: Take about 250 g of mixed bed resin and add it into the first-stage resin separation column 1.

[0030] Step 3: The computer 7 sends a command to the controller 6, and then the controller 8 sends the command to the circulation pump 4, and the circulation pump 4 starts to rotate at a relatively high speed, so that the demineralized water continuously enters the first-stage resin separation column 1. At this time, the mixed bed ion exchange resin begins to disperse in the first-stage resin separation column 1 under the impact of the high-speed water flow, and gradually enters a fluidized state.

[0031] Step 4: After 10 minutes, the ion exchange resin is completely dispersed. At this time, the circulation pump 4 starts to rotate at a relatively low speed until the first-stage resin separation column 1 is gradually filled with deionized water. At this time, the deionized water mixed with the ion exchange resin overflows into the second-stage resin separation column 2 through the overflow port at the top of the first-stage resin separation column 1; Step 5: As the second-stage resin separation column 2 is also filled with deionized water mixed with ion exchange resin, the deionized water mixed with ion exchange resin begins to overflow to the third-stage resin separation column 3 through the overflow port.

[0032] Step 6: As the third-stage resin separation column 3 is filled, the deionized water mixed with the ion exchange resin eventually overflows into the anion exchange resin collector 12; a sand core filter plate 8 is installed in the middle of the anion exchange resin collector 12 to separate the anion exchange resin and the deionized water; a weight sensor 9 is installed at the bottom of the sand core filter plate 8, and a liquid level sensor 10 is installed in the middle of the anion exchange resin collector 12; when the mass of the anion exchange resin on the upper part of the sand core filter plate 8 is greater than 100g or the liquid level reaches the maximum liquid level of 15cm, the data is transmitted back to the controller 6 and fed back to the computer 7; Step 7: The computer 7 sends a command to the controller 6, the circulation pump 4 stops rotating, and at the same time the solenoid valve 11 at the bottom of the anion exchange resin collector opens, and the deionized water circulates into the deionized water tank 5.

[0033] Step 8: Take out the anion exchange resin from the upper part of the anion resin collector 12 , and take out the cation exchange resin from the lower part of the first-stage resin separation column 1 .

[0034] Example 1 Step 1: Fill the desalted water tank 5 with desalted water; Step 2: Take about 250g of mixed bed resin (001×7MB, 201×7MB) and add it to the first-stage resin separation column 1; Step 3: Use the computer 7 to send instructions to the controller 6, and then the controller 6 sends instructions to the circulation pump 4, and the circulation pump 4 starts to rotate at speeds of 50r / min, 100r / min, 150r / min, 200r / min, and 250r / min, respectively, so that the desalted water continuously enters the first-stage resin separation column 1; Step 4: Observe the dispersion of the resin under different pump speeds. It was found that when the pump speed is 50r / min, 100r / min, and 150r / min, the resin is difficult to be completely separated in the first-stage resin separation column 1 due to the small water flow rate. When the pump speed is 250r / min, the desalted water flow rate is too large, and the cation exchange resin also enters the second-stage resin separation column 2 along with the desalted water. Therefore, the initial speed of the circulation pump is determined to be 200r / min.

[0035] Example 2 Step 1: Fill the desalted water tank 5 with desalted water.

[0036] Step 2: Take about 250g of mixed bed resin (001×7MB, 201×7MB, such as Figure 2 As shown) is added into the first-stage resin separation column 1; Step 3: The computer 7 sends a command to the controller 6, and then the controller 6 sends the command to the circulation pump 4, and the circulation pump 4 starts to rotate at a speed of 200 r / min, so that the desalted water continuously enters the first-stage resin separation column 1, and the mixed bed resin is gradually dispersed in the first-stage resin separation column 1 under the impact of the high-speed water flow; Step 4: After 10 minutes, the resin is completely dispersed. At this time, in order to prevent the flow rate from being too fast and causing a large amount of cationic resin to enter the second-stage resin separation column 2, the circulation pump speed is adjusted to 150r / min. At this time, it can be observed that most of the cation exchange resin is concentrated in the lower part of the first-stage resin separation column 1, while most of the anion exchange resin is concentrated in the upper part of the first-stage resin separation column 1, but the two are not completely separated; Step 5: As the circulation pump 4 continues to work, the deionized water doped with ion exchange resin on the top of the first-stage resin separation column 1 begins to enter the second-stage resin separation column 2 for the second separation of anion exchange resin and cation exchange resin. At this time, the cation exchange resin in the second-stage resin separation column 2 has been significantly reduced, and most of it is anion exchange resin; Step 6: As the second-stage resin separation column 2 is filled, the deionized water doped with ion exchange resin in the upper part of the second-stage resin separation column 2 begins to enter the third-stage resin separation column 3 for the third separation of anion exchange resin and cation exchange resin. At this time, the third-stage resin separation column 3 contains only a small amount of cation exchange resin, and the vast majority is anion exchange resin; Step 7: As the third-stage resin separation column 3 is filled, the deionized water doped with anion exchange resin in the upper portion of the third-stage resin separation column 3 begins to enter the anion exchange resin collector 12; at this time, since the deionized water contains a small amount of anion exchange resin, the liquid level in the anion exchange resin collector 12 quickly reaches the maximum liquid level; Step 8: The electromagnetic valve at the bottom of the anion exchange resin collector 12 is opened, and the deionized water enters the deionized water tank to continue resin separation. After all the deionized water at the bottom of the anion exchange resin collector 12 enters the deionized water tank, the electromagnetic valve is closed; Step 9: With the continuous circulation of desalted water, the anion exchange resin on the sand core filter plate of the anion exchange resin collector 12 reaches 100g, at which time the circulation pump 4 stops working; the anion exchange resin is taken out from the upper part of the anion exchange resin collector 12 as shown in FIG. Figure 3 As shown, a cation exchange resin is taken out from the bottom of the first-stage resin separation column 1. Figure 4 shown.

[0037] The above contents are only for explaining the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. Any changes made on the basis of the technical solution in accordance with the technical idea proposed by the present invention shall fall within the protection scope of the claims of the present invention.

Claims

1. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device, characterized in that: It includes a desalted water tank (5), a circulation pump (4), a multi-stage resin separation column system, an anion resin collection system and a control system; One end of the desalted water tank (5), the circulation pump (4), the multi-stage resin separation column system and one end of the anion resin collection system are connected in sequence, and the other end of the desalted water tank (5) and the other end of the anion resin collector (12) are connected to form a circulation loop; The circulation pump (4) and the anion resin collection system are respectively connected to a control system.

2. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device according to claim 1, characterized in that: The multi-stage resin separation column system comprises a first-stage resin separation column (1), a second-stage resin separation column (2) and a third-stage resin separation column (3) which are connected in sequence; The first-stage resin separation column (1) is connected to a circulation pump (4); and the third-stage resin separation column (3) is connected to an anion resin collection system.

3. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device according to claim 2, characterized in that: The anion resin collection system comprises a sand core filter plate (8), a mass sensor (9), a liquid level sensor (10) and an anion resin collector (12); the two ends of the anion resin collector (12) are respectively connected to a third-stage resin separation column (3) and a demineralized water tank (5); the sand core filter plate (8) is arranged inside the anion resin collector (12); and the mass sensor (9) and the liquid level sensor (10) are both arranged below the sand core filter plate (8).

4. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device according to claim 3, characterized in that: The control system comprises a controller (6) and a computer (7) which are connected to each other; the mass sensor (9) and the liquid level sensor (10) are both connected to the controller (6).

5. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device according to claim 4, characterized in that: A solenoid valve (11) is also provided on the pipeline connecting the desalted water tank (5) and the anion resin collector (12).

6. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation device according to claim 5, characterized in that: The solenoid valve (11) is connected to the controller (6).

7. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method, characterized in that: The method is implemented by using the device described in any one of claims 1 to 6, comprising the following steps: First, desalted water is added to the desalted water tank (5), and then mixed bed resin is added to the multi-stage resin separation column system; The control system sends instructions to the circulation pump (4) to continuously allow desalted water to enter the multi-stage resin separation column system, so that the mixed bed resin enters a fluidized state; then the control system controls the circulation pump (4) so ​​that the multi-stage resin separation column system obtains desalted water mixed with ion exchange resin, and enters the anion resin collection system to obtain anion exchange resin and desalted water.

8. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method according to claim 7, characterized in that: The anion resin collection system comprises an anion resin collector (12); The control system comprises a controller (6) and a computer (7) connected to each other; When performing separation, the following steps are specifically included: The computer (7) sends instructions to the controller (6), and the controller (6) sends the instructions to the circulation pump (4), and the circulation pump (4) starts to rotate, so that the desalted water continuously enters the first-stage resin separation column (1), and the mixed bed ion exchange resin in the mixed bed resin gradually enters a fluidized state; After the mixed bed ion exchange resin in the mixed bed resin is completely dispersed, the circulation pump (4) adjusts its rotation speed until the deionized water in the first-stage resin separation column (1) is filled, and then the deionized water mixed with the ion exchange resin overflows into the second-stage resin separation column (2); as the deionized water mixed with the ion exchange resin in the second-stage resin separation column (2) is filled, the deionized water mixed with the ion exchange resin overflows into the third-stage resin separation column (3); as the third-stage resin separation column (3) is filled, the deionized water mixed with the ion exchange resin finally overflows into the anion exchange resin collector (12).

9. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method according to claim 8, characterized in that: The anion resin collection system further comprises a sand core filter plate (8), a mass sensor (9), and a liquid level sensor (10); a solenoid valve (11) is also provided on the pipeline connecting the desalted water tank (5) and the anion resin collector (12); when separation is performed, the following steps are specifically included: The deionized water mixed with the ion exchange resin flowing into the anion exchange resin collector (12) is separated into the anion exchange resin and the deionized water by the sand core filter plate (8); when the level of the anion exchange resin or the deionized water on the upper part of the sand core filter plate (8) reaches the standard, it is fed back to the controller (6) and then to the computer (7); The computer (7) issues a command to the controller (6), the circulation pump (4) stops rotating, and the solenoid valve (11) at the bottom of the anion exchange resin collector opens, and the deionized water circulates into the deionized water tank (5); Anion exchange resin is taken out from the upper part of the anion resin collector (12), and cation exchange resin is taken out from the lower part of the first-stage resin separation column (1).

10. A laboratory multi-stage countercurrent water inflow mixed bed resin complete separation method according to claim 9, characterized in that: The standard for the level of the anion exchange resin or deionized water on the upper part of the sand core filter plate (8) is: the mass of the anion exchange resin is greater than 100 g or the level of the deionized water reaches 15 cm.

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