Apparatus and method for batch determination of moisture content of hydroxyl form anion exchange resin
Through the device design of transformation reaction tank, peristaltic pump and pH online monitor, the cumbersomeness and instability problems of measuring the water content of hydroxyl type anion exchange resin are solved, efficient and accurate batch measurement is achieved, and reagent consumption is reduced.
Patent Information
- Application Number
- CN202510236554.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2045-02-28
AI Technical Summary
The existing method for determining the water content of hydroxyl anion exchange resin is cumbersome, the weighing results are unstable, the reagent consumption is large, and the accuracy is insufficient, making batch determination impossible.
The device design adopts a transformation reaction tank, peristaltic pump and pH online monitor. The sample is weighed, transformed and dried through a basket structure. The peristaltic pump is used to control the solution flow and the pH monitoring is used to determine the completion of the reaction, reducing reagent consumption and improving the degree of automation.
The accurate and stable determination of the water content of the hydroxide anion exchange resin is achieved, the reagent consumption is reduced, the automation degree of the determination results and the experimental efficiency are improved, and the weighing error is avoided.
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Figure CN119861004B_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the field of water content testing of anion exchange resins, and in particular to a device and method for batch testing the water content of hydroxyl type anion exchange resins. Background Art
[0002] The moisture content of ion exchange resins refers to the internal moisture content of the resin particles after removing external free water. It is a key property of resin products. The moisture content of ion exchange resins is related to factors such as the resin type, structure, acidity, degree of crosslinking, exchange capacity, and ion form. If the resin undergoes chain breakage, changes in pore structure, or a decrease in exchange capacity during use, its moisture content will also change accordingly. Therefore, changes in the moisture content of ion exchange resins can also reflect changes in their inherent performance.
[0003] The conventional method for determining the moisture content of ion exchange resins is to remove free water from the resin by centrifugation, then weigh a certain mass of the sample and dry it in an oven at (105±3)°C. Finally, the moisture content is calculated based on the change in mass. However, for hydroxide-type anion exchange resins, their strong base groups are susceptible to thermal degradation at temperatures above 80°C, making the direct drying method ineffective for determining moisture content.
[0004] The currently disclosed method for measuring the water content of hydrogen-oxygen type anion exchange resin is to test according to GB / T 5759-2000 “Method for measuring the water content of oxygen-oxygen type anion exchange resin”. The prepared hydrogen-oxygen type anion exchange resin sample is accurately weighed and placed in a constant weight water content tester. The water content tester is a small glass chromatographic column. The sample is completely converted into a chlorine type by using a quantitative hydrochloric acid through the ion exchange resin layer. After the excess hydrochloric acid is removed by using anhydrous ethanol, the water content tester and the resin sample are placed in an oven at (105±3) DEG C for drying. The dry basis mass of the chlorine type is measured. The dry basis mass of the hydrogen-oxygen type sample is calculated by subtracting the mass increment generated in the conversion process. Finally, the water content is calculated. This method can effectively solve the problem of measuring the water content of hydrogen-oxygen type anion exchange resin. However, it also has the following disadvantages: 1. It relies on manual operation, the process is relatively complicated, and it consumes a lot of manpower; 2. After the ion exchange resin is converted, it is difficult to completely transfer out of the water content tester. Therefore, the water content tester is placed on an electronic balance together with the water content tester before and after the conversion. The length of the water content tester exceeds the weighing pan of the common electronic balance, and the shape is not uniform. The weighing result is unstable due to the influence of the placement position; 3. There is a space between the lower part of the sand core of the water content tester and the piston. Liquid is easily accumulated in this space. If the accumulated liquid is not completely evaporated during the drying process in the oven, it will seriously affect the accuracy of the measurement result; 4. In order to ensure complete conversion, about 1 g of single ion exchange resin sample needs to use 200 mL to 250 mL of hydrochloric acid for conversion, which consumes a large amount of reagent. SUMMARY
[0005] In view of the problems in the prior art, the present application provides a device and method for batch measuring the water content of hydrogen-oxygen type anion exchange resin, to solve the problems of the traditional chromatographic column type water content tester, such as complicated process, unstable weighing result, high accuracy and large amount of hydrochloric acid consumption. The device has high automation degree and convenient operation, can batch process the anion exchange resin sample, reduces the reagent consumption, eliminates the weighing error, and has better stability and accuracy of the result.
[0006] The present application is realized by the following technical solutions.
[0007] A device for batch measuring the water content of hydrogen-oxygen type anion exchange resin, comprising a conversion reaction tank, an inlet peristaltic pump, an outlet peristaltic pump and a pH online monitor.
[0008] A plurality of mesh baskets are placed in the conversion reaction tank, and each mesh basket is used for placing the hydrogen-oxygen type anion exchange resin to be measured.
[0009] A liquid storage tank is communicated with the end of the inlet pipeline on one side of the conversion reaction tank, and the inlet peristaltic pump is installed on the inlet pipeline.
[0010] The other side of the transformation reaction tank is communicated with a waste liquid recovery tank through the end of an outlet pipeline, an outlet peristaltic pump and a pH online monitor are installed on the outlet pipeline, and the pH online monitor is arranged close to the waste liquid recovery tank.
[0011] Preferably, the slot of the transformation reaction tank is provided with a top cover, the basket is a cylindrical structure and is provided with a protruding structure at the top, a plurality of circular holes are formed in the top cover, the diameter of the circular holes is greater than the diameter of the cylindrical wall of the basket and is less than the diameter of the top protrusion of the basket.
[0012] Preferably, the bottom and the cylindrical wall of the basket are provided with through holes, and the through holes can prevent the hydrogen-oxygen type anion exchange resin to be determined from leaking out of the basket.
[0013] A method for batch determination of the water content of hydrogen-oxygen type anion exchange resin, based on the test device for the water content of hydrogen-oxygen type anion exchange resin according to any one of the preceding claims, comprising the following steps:
[0014] S1, a plurality of baskets containing the hydrogen-oxygen type anion exchange resin to be determined are placed in the transformation reaction tank, the outlet peristaltic pump is closed, the inlet peristaltic pump is opened to flow hydrochloric acid into the transformation reaction tank, the outlet peristaltic pump is opened when the liquid level exceeds the anion exchange resin in the basket, and the flow rates of the inlet peristaltic pump and the outlet peristaltic pump are adjusted to be consistent, and the solution in the transformation reaction tank flows out to the waste liquid recovery tank through the outlet pipeline, the outlet peristaltic pump and the pH online monitor;
[0015] S2, the reading of the pH online monitor is observed, the inlet peristaltic pump is closed when the anion exchange resin has been converted into the chlorine type, and the remaining hydrochloric acid in the transformation reaction tank is discharged;
[0016] S3, the outlet peristaltic pump is closed, the inlet peristaltic pump is opened to introduce anhydrous ethanol into the transformation reaction tank, the outlet peristaltic pump is opened when the liquid level exceeds the anion exchange resin in the basket, and the effluent flows out to the waste liquid recovery tank through the outlet pipeline, the outlet peristaltic pump and the pH online monitor, and the process is stopped when the pH is 7, and all the baskets are taken out for drying;
[0017] S4, the water content of the hydrogen-oxygen type anion exchange resin to be determined in each basket is calculated according to the mass of each basket in S1, the initial total mass of each basket containing the anion exchange resin, the total mass of each basket of the anion exchange resin after drying in S3, and the wet basis total exchange capacity and the wet basis strong base group capacity of the anion exchange resin in each basket.
[0018] Preferably, in S1, the outlet peristaltic pump is opened when the liquid level exceeds the anion exchange resin in the basket by 1-2 cm.
[0019] Preferably, in S1, the flow rates of the inlet peristaltic pump and the outlet peristaltic pump are both 10 mL / min to 20 mL / min.
[0020] Preferably, the concentration of the hydrochloric acid in S1 is 1 mol / L to 2 mol / L.
[0021] Preferably, in S2, when the pH value of the pH online monitor rises and then drops to a constant value, the anion exchange resin is converted into the chloride type after continuously introducing hydrochloric acid for 10 min to 15 min.
[0022] Preferably, in S3, when the liquid level exceeds the anion exchange resin in the basket, the outlet peristaltic pump is turned on, and the flow rates of the inlet peristaltic pump and the outlet peristaltic pump are adjusted to 8 mL / min to 16 mL / min.
[0023] Preferably, S4 calculates the water content of the hydroxide-type anion exchange resin to be measured in each basket according to the following formula:
[0024] ;
[0025] X - the water content of the corresponding hydroxyl anion exchange resin to be determined in each basket in S1, expressed as a percentage;
[0026] m 1—the mass of each basket in S1, in g;
[0027] m 2—the total mass of each basket containing the anion exchange resin in S1, in g;
[0028] m 3—Total mass of each basket containing dried anion exchange resin in S3, in g;
[0029] E 1—Wet basis total exchange capacity of the corresponding hydroxide anion exchange resin in each basket in S1, in mmol / g;
[0030] E 2—Wet-basis strong base group capacity of the corresponding hydroxide-type anion exchange resin in each basket of S1, in mmol / g.
[0031] Compared with the prior art, the present invention has the following beneficial technical effects:
[0032] The application discloses a device for batch determination of water content of hydroxyl type anion exchange resin, which adopts a basket structure design and has the characteristics of simple structure and small size. The device can directly put the hydroxyl type anion exchange resin sample to be determined into the weighing pan of a balance for weighing, overcomes the problem of unstable weighing result of a traditional water content determinator, avoids the weighing error, and makes the determination result more accurate. Before a transformation process of the hydroxyl type anion exchange resin sample, a plurality of baskets can be inserted into a transformation reaction tank. During the transformation process, the through holes of the baskets can make the solution in the reaction tank enter and react with the sample, and the sample particles cannot leak out. After the transformation reaction is completed, the excess acid is washed away with anhydrous ethanol, and then the sample is placed in an oven for drying, thereby completing the main steps of weighing, batch exchange transformation and drying. During the transformation reaction process, the acidity of the effluent is determined by a pH on-line monitor, and when the pH value is stable and unchanged, it can be judged that the reaction is complete, the hydroxyl type anion exchange resin sample has been completely transformed into a chlorine type, and the input of hydrochloric acid is stopped, thereby saving the reagent consumption. The reaction solution is automatically input and output by a peristaltic pump, and compared with the traditional method of adding the solution by a separatory funnel, the flow can be automatically and effectively controlled, on the one hand, the consumption of hydrochloric acid for transformation is saved, and on the other hand, the concentration of the hydrochloric acid in contact with the ion exchange resin sample is maintained, so that the equilibrium reaction can continuously proceed in a positive direction. The device has high automation degree and convenient operation, and compared with the traditional device, the device has smaller reagent consumption, eliminates the weighing error, has better stability and accuracy of the result, realizes batch transformation treatment of the anion exchange resin sample, and further determines the water content.
[0033] The present invention provides a method for batch determination of the water content of hydroxyl-type anion exchange resins. The ion exchange resin sample can be placed in a mesh basket with through holes for weighing, transformation reaction, and drying. During the transformation process, a dynamic immersion exchange method is used, and hydrochloric acid or anhydrous ethanol is injected into the transformation reaction tank through an inlet pipe by an inlet peristaltic pump. The transformation and water washing progress can be accurately and quickly determined by an online pH monitor. The outflowing liquid is injected into a recovery tank through an outlet pipe and an online pH monitor by an outlet peristaltic pump. The peristaltic pump automatically inputs and outputs the reaction solution, and compared with the traditional method of adding the solution using a separatory funnel, the flow rate can be automatically and effectively controlled. On the one hand, the consumption of hydrochloric acid for transformation is saved, and on the other hand, the concentration of hydrochloric acid in contact with the hydroxyl-type anion exchange resin sample is maintained, so that the equilibrium reaction can continue in the positive direction. After the hydroxyl-type anion exchange resin is converted to the chloride type, anhydrous ethanol is added to wash away excess acid, thereby ensuring the accuracy of the measurement results. The use of a mesh basket for pre- and post-weighing and drying ensures the consistency of the measurement conditions, and the calculated mass difference is more accurate. Finally, the mass of the mesh basket, the initial total mass of the mesh basket containing the anion exchange resin, the total mass of the mesh basket containing the transformed anion exchange resin after drying, and the wet-based total exchange capacity and wet-based strong base group capacity of the anion exchange resin can be used to accurately calculate the water content of the hydroxyl anion exchange resin to be measured in each mesh basket in batches. In summary, the method of the present invention has a higher degree of automation than the traditional method, consumes less reagents, and has higher experimental efficiency. It avoids the problem of unstable weighing results caused by the large size and irregular shape of the traditional water content meter. In addition, it has the advantages of rigorous process, controllable conditions, and accurate and reliable results. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 This is a schematic diagram of the device for batch determination of water content of hydroxyl-type anion exchange resins according to the present invention.
[0035] Figure 2 for Figure 1 Partial cross-sectional view of the middle basket.
[0036] Figure 3 for Figure 1 Schematic diagram of the structure of the middle basket.
[0037] In the figure: transformation reaction tank 1, top cover 2, mesh basket 3, liquid inlet 4, inlet pipeline 5, inlet peristaltic pump 6, liquid outlet 7, outlet pipeline 8, outlet peristaltic pump 9, pH online monitor 10, waste liquid recovery tank 11, liquid storage tank 12. DETAILED DESCRIPTION
[0038] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments and drawings, which are intended to explain rather than limit the present invention.
[0039] The present invention provides a device for batch determination of water content of hydroxyl type anion exchange resin, such as Figure 1 As shown, a plurality of mesh baskets 3 are evenly placed in the transition reaction tank 1 through the top cover 2, and the hydroxide-type anion exchange resin to be measured is placed in the mesh baskets 3. The transition reaction tank 1 is in the shape of a rectangular parallelepiped, and the top cover 2 is a support plate of a certain thickness and matches the shape of the notch of the transition reaction tank 1. The top cover 2 is inserted into the notch of the transition reaction tank 1 and the upper surfaces of the two are flush, so the top cover 2 is detachable. The mesh basket 3 is a cylindrical structure, and a plurality of circular holes are opened in the top cover 2, so that the mesh basket 3 can be vertically placed into the transition reaction tank 1 through the corresponding holes, and the top protrusion is hung on the top cover 2.
[0040] A liquid inlet 4 is provided on one side of the upper outer wall of the transformation reaction tank 1. An inlet peristaltic pump 6 is connected to the liquid inlet 4 via an inlet pipe 5. The end of the inlet pipe 5 is inserted into a liquid storage tank 12. The liquid storage tank 12 can contain hydrochloric acid or anhydrous ethanol, so that the corresponding liquid can be added to the transformation reaction tank 1 through the inlet peristaltic pump 6. A liquid outlet 7 is provided on the other side of the lower outer wall of the transformation reaction tank 1. The liquid outlet 7, the outlet peristaltic pump 9, and the pH online monitor 10 are connected via an outlet pipe 8. The end of the outlet pipe 8 is inserted into a waste liquid recovery tank 11, so that the outflowing liquid can enter the waste liquid recovery tank 11.
[0041] The height of the transformation reaction tank 1 is 5 cm to 10 cm, and the material is acid corrosion resistant material such as polymethyl methacrylate or glass. The specific structure of the basket 3 is as follows: Figure 3 As shown, a raised structure is provided on the top of the cylinder, and the diameter of the circular through hole in the top cover 2 is 0.5-1 mm larger than the cylinder of the net basket 3 and 1-3 mm smaller than the raised portion on the top of the net basket 3. In this way, the net basket 3 can be inserted into the transformation reaction tank 1 through the hole in the top cover 2 without falling in, and the bottom of the raised portion is flush with the upper surface of the notch of the transformation reaction tank 1.
[0042] The basket 3 is a mesh or full of strip-shaped through holes. The specific through hole structure design of the basket 3 can be as follows: Figure 2 As shown, through-holes are provided on both the bottom and the wall of the basket to allow liquid to quickly flow in and out of the basket. The through-holes are evenly distributed in a long strip shape, ranging from 1 mm to 2 mm in length and 0.10 mm to 0.20 mm in width. This width is smaller than the diameter of the ion exchange resin. This allows the solution in the transition reaction tank 1 to contact the sample inside the basket 3 and prevents the hydroxide-type anion exchange resin to be measured from leaking out of the basket 3. The bottom diameter of the basket 3 is 2 cm to 3 cm, and the height is 2 cm to 5 cm. A raised curved handle is provided for easy handling. The material is heat-resistant and acid-resistant, such as polytetrafluoroethylene or phenolic resin.
[0043] The present invention provides a method for batch determination of the water content of hydroxyl-type anion exchange resin, based on the above-mentioned testing device, comprising the following steps:
[0044] In the first step, all the baskets 3 were cleaned and dried in an oven at (105±3)℃ to constant weight. The weights of the baskets were weighed. m 1;
[0045] In the second step, the free water outside the hydroxyl anion exchange resin sample to be tested is removed by centrifugation. 2 g to 4 g of the ion exchange resin sample is weighed using an electronic balance and placed in the basket 3 that has been weighed constant in the first step. The total mass of the sample and the basket 3 is read. m 2;
[0046] In the third step, the mesh basket 3 containing the hydroxide-type anion exchange resin sample is placed into the transformation reaction tank 1 through the top cover 2, and the top protrusion is suspended on the top cover 2. The outlet peristaltic pump 9 is closed, and the inlet pipe 5 is connected to 1 mol / L~2 mol / L hydrochloric acid. The hydrochloric acid is flowed into the transformation reaction tank 1 through the liquid inlet 4 by the inlet peristaltic pump 6. When the liquid level exceeds the ion exchange resin layer in the mesh basket 3 by 1 cm~2 cm (the volume of the transformation reaction tank 1 can be calculated by the flow rate of the inlet peristaltic pump 6 and the height of the sample), the outlet peristaltic pump 9 is turned on, and the flow rates of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 are adjusted to be consistent, at 10 mL / min~20 mL / min. The solution in the transformation reaction tank 1 flows out to the waste liquid recovery tank 11 through the liquid outlet 7, the outlet pipe 8, the outlet peristaltic pump 9, and the pH online monitor 10;
[0047] Step 4: Observe the reading of the pH online monitor 10. When the pH value of the outlet solution rises and then drops to a constant value, continue to introduce hydrochloric acid for 10 to 15 minutes to ensure that the transformation reaction is complete. Turn off the inlet peristaltic pump 6 and drain the remaining hydrochloric acid in the transformation reaction tank 1. At this time, the hydroxide-type anion exchange resin sample has been converted to the chloride-type.
[0048] Step 5: Close the outlet peristaltic pump 9, connect the inlet pipe 5 to anhydrous ethanol, and use the inlet peristaltic pump 6 to let the anhydrous ethanol flow into the transformation reaction tank 1 through the liquid inlet 4. When the liquid level exceeds the ion exchange resin layer in the basket 3 by 1 cm to 2 cm, start the outlet peristaltic pump 9. At the same time, adjust the flow rate of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 to be consistent, at 8 mL / min to 16 mL / min. The outlet outflow solution flows into the waste liquid recovery tank 11. When the pH of the outlet outflow solution reaches 7, stop. At this time, the excess hydrochloric acid in the anion exchange resin has been washed away, and the outflow solution is neutral.
[0049] Step 6: Take out the basket 3 containing the anion exchange resin sample, place it on a tray and put it into a preheated constant temperature drying oven, and dry it at (105±3)℃ for 2 hours;
[0050] Step 7: After drying, place the basket 3 containing the anion exchange resin sample in a desiccator, cool it to room temperature, and weigh the mass after drying. m 3;
[0051] Step 8: Determine the wet basis full exchange capacity of the anion exchange resin according to GB / T5760 "Determination of exchange capacity of hydroxyl type anion exchange resin" E 1 and wet base strong base group capacity E 2. Used to calculate the quality increment generated by the transformation process;
[0052] In the ninth step, the water content of the hydroxide-type anion exchange resin is calculated according to the following formula (1).
[0053] (1)
[0054] in:
[0055] X —water content, expressed as a percentage;
[0056] m 1—the mass of the basket in the first step, in g;
[0057] m 2—Total mass of the ion exchange resin sample and basket in the second step, in grams;
[0058] m 3—Total mass of the ion exchange resin sample and basket after drying in step 7, in g;
[0059] E 1—Wet basis total exchange capacity of anion exchange resin, in mmol / g;
[0060] E 2—Wet basis strong base group capacity of the anion exchange resin, in mmol / g.
[0061] Example 1
[0062] The present invention provides a method for batch determination of water content of hydroxide-type anion exchange resin, which specifically comprises the following steps:
[0063] The first step is to clean and number the eight baskets 3, dry them in an oven at 105°C to constant weight, and weigh the mass of each basket. m 1i , i=1~8;
[0064] In the second step, remove the external free water of 8 unused hydroxyl anion exchange resins by centrifugation. Weigh (3.0-3.1) g of ion exchange resin samples using an electronic balance and place them in the basket 3 that has been weighed in the first step. Read the total mass of the ion exchange resin sample and basket 3. m 2i , i=1~8;
[0065] In the third step, eight mesh baskets 3 containing hydroxyl anion exchange resin samples were respectively inserted into the transformation reaction tank 1 through the top cover 2, the outlet peristaltic pump 9 was closed, the inlet pipe 5 was connected to 1 mol / L hydrochloric acid, and the hydrochloric acid was flowed into the transformation reaction tank 1 through the liquid inlet 4 by the inlet peristaltic pump 6. When the liquid level exceeded the ion exchange resin layer in the mesh basket 3 by 1 cm, the outlet peristaltic pump 9 was turned on, and the flow rate of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 was adjusted to be consistent at 15 mL / min. The solution in the transformation reaction tank 1 passed through the liquid outlet 7, the outlet pipe 8, the outlet peristaltic pump 9, and the pH online monitor 10 and then flowed out to the waste liquid recovery tank 11;
[0066] Step 4: Observe the reading of the pH online monitor 10. When the pH value of the outlet solution rises and then drops to a constant value, continue to introduce 1 mol / L hydrochloric acid for 10 minutes and then turn off the inlet peristaltic pump 6 to ensure that the transformation reaction is complete and discharge the remaining hydrochloric acid in the transformation reaction tank 1. At this time, the hydroxide-type anion exchange resin sample has been converted to the chloride-type.
[0067] Step 5: Close the outlet peristaltic pump 9, connect the inlet pipe 5 to anhydrous ethanol, and use the inlet peristaltic pump 6 to let the anhydrous ethanol flow into the transformation reaction tank 1 through the liquid inlet 4. When the liquid level exceeds the ion exchange resin layer in the basket 3 by 1 cm, start the outlet peristaltic pump 9. At the same time, adjust the flow rate of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 to be consistent, which is 12 mL / min. The outlet solution flows into the waste liquid recovery tank 11. When the outlet solution is neutral, stop, and the excess hydrochloric acid in the anion exchange resin has been washed away.
[0068] Step 6: Take out 8 mesh baskets 3, place them on a tray and put them into a preheated constant temperature drying oven, and bake them at (105±3)°C for 2 hours;
[0069] Step 7: After drying, place the 8 baskets 3 containing the anion exchange resin samples in a desiccator, cool to room temperature, and weigh the mass after drying. m 3i , i=1~8;
[0070] Step 8: Determine the wet basis full exchange capacity of the anion exchange resin according to GB / T5760 "Determination of exchange capacity of hydroxyl type anion exchange resin" E 1i(i=1~8) and wet base strong base group capacity E 2i (i=1~8), used to calculate the mass increment generated by the transformation process;
[0071] The ninth step is to calculate the water content of the eight hydroxide-type anion exchange resins. The results are shown in Table 1.
[0072] Table 1 Water content measurement data
[0073]
[0074] The moisture content of unused hydroxyl-type anion exchange resin samples is generally between 50% and 60%. The resin samples in Table 1 all have moisture contents between 50% and 60%, indicating reasonable determination results. The moisture content of the eight samples in the first step was determined using the current standard method GB / T 5759-2000, "Determination of Moisture Content of Hydroxy-Type Anion Exchange Resins," and compared with the moisture content results in Table 1. The absolute difference between the two methods was 0.1% to 1.0%, indicating that this method is accurate.
Claims
1. A method for batch determination of water content of hydroxide-type anion exchange resin, characterized in that: A device for testing the water content of a hydroxy-type anion exchange resin, the device comprising a transformation reaction tank (1), an inlet peristaltic pump (6), an outlet peristaltic pump (9) and a pH online monitor (10); A plurality of mesh baskets (3) are placed in the transformation reaction tank (1), and each mesh basket (3) is used to place a hydroxide-type anion exchange resin to be measured; One side of the transformation reaction tank (1) is connected to a liquid storage tank (12) through the end of an inlet pipeline (5), and an inlet peristaltic pump (6) is installed on the inlet pipeline (5); The other side of the transformation reaction tank (1) is connected to a waste liquid recovery tank (11) through the end of the outlet pipe (8), and the outlet peristaltic pump (9) and the pH online monitor (10) are installed on the outlet pipe (8), and the pH online monitor (10) is arranged close to the waste liquid recovery tank (11); The specific steps include: S1, placing a plurality of mesh baskets (3) containing the hydroxyl type anion exchange resin to be measured in the transformation reaction tank (1), closing the outlet peristaltic pump (9), opening the inlet peristaltic pump (6) to flow hydrochloric acid into the transformation reaction tank (1), opening the outlet peristaltic pump (9) when the liquid level exceeds the anion exchange resin in the mesh basket (3), and adjusting the flow rates of the inlet peristaltic pump (6) and the outlet peristaltic pump (9) to be consistent, and the solution in the transformation reaction tank (1) flows out to the waste liquid recovery tank (11) after passing through the outlet pipe (8), the outlet peristaltic pump (9) and the pH online monitor (10); S2, observing the reading of the pH online monitor (10), when the anion exchange resin has been converted into the chloride type, closing the inlet peristaltic pump (6) to discharge the remaining hydrochloric acid in the transformation reaction tank (1); S3, close the outlet peristaltic pump (9), open the inlet peristaltic pump (6) to connect anhydrous ethanol to the transformation reaction tank (1), and open the outlet peristaltic pump (9) when the liquid level exceeds the anion exchange resin in the mesh basket (3). The outflow liquid flows through the outlet pipe (8), the outlet peristaltic pump (9) and the pH online monitor (10) and then flows into the waste liquid recovery tank (11). When the pH reaches 7, stop, and take out all the mesh baskets (3) for drying; S4, calculating the water content of the hydroxyl anion exchange resin to be measured in each basket (3) based on the mass of each basket (3) in S1, the initial total mass of each basket (3) containing the anion exchange resin, the total mass of each basket (3) of the anion exchange resin after drying in S3, and the wet basis total exchange capacity and wet basis strong base group capacity of the anion exchange resin in each basket (3).
2. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: The slot of the transformation reaction tank (1) is provided with a top cover (2), the mesh basket (3) is a cylindrical structure and is provided with a convex structure on the top, and a plurality of circular holes are opened in the top cover (2), the diameter of the circular holes is larger than the diameter of the cylinder wall of the mesh basket (3) and smaller than the diameter of the top convex of the mesh basket (3).
3. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: The bottom and the wall of the mesh basket (3) are provided with through holes, and the through holes can prevent the hydroxyl type anion exchange resin to be measured from leaking out of the mesh basket (3).
4. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: In S1, when the liquid level exceeds the anion exchange resin in the basket (3) by 1 cm to 2 cm, the outlet peristaltic pump (9) is turned on.
5. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: In S1, the flow rates of the inlet peristaltic pump (6) and the outlet peristaltic pump (9) are both 10 mL / min to 20 mL / min.
6. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: The concentration of the hydrochloric acid in S1 is 1 mol / L to 2 mol / L.
7. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 6, characterized in that: In S2, when the pH value of the pH online monitor (10) rises and then falls to a constant value, the anion exchange resin is converted into the chloride type after continuously introducing hydrochloric acid for 10 min to 15 min.
8. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: In S3, when the liquid level exceeds the anion exchange resin in the basket (3), the outlet peristaltic pump (9) is turned on, and the flow rates of the inlet peristaltic pump (6) and the outlet peristaltic pump (9) are adjusted to 8 mL / min to 16 mL / min.
9. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 1, characterized in that: S4 calculates the water content of the hydroxyl anion exchange resin to be measured in each basket (3) according to the following formula: ; X - the water content of the corresponding hydroxyl anion exchange resin to be determined in each basket (3) in S1, expressed as a percentage; m 1—mass of each basket (3) in S1, in g; m 2—the total mass of each basket (3) containing the anion exchange resin in S1, in g; m 3—total mass of each basket (3) containing dried anion exchange resin in S3, in g; E 1—the wet basis total exchange capacity of the corresponding hydroxyl anion exchange resin in each basket (3) in S1, in mmol / g; E 2—Wet-basis strong base group capacity of the corresponding hydroxide-type anion exchange resin in each basket (3) in S1, in mmol / g.
Citation Information
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