Device and method for measuring water content of oxyhydrogen type anion exchange resin in batches
By designing a batch measurement device using a basket structure and dynamic immersion exchange method, the problems of cumbersome operations, unstable results and high reagent consumption in the water content measurement method of hydroxide-type anion exchange resin are solved, and high accuracy and high efficiency water content measurement is achieved.
Patent Information
- Application Number
- CN202510236554.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2025-04-22
- Estimated Expiration
- 2045-02-28
AI Technical Summary
In the prior art, the method for measuring the moisture content of the hydroxide-type anion exchange resin has problems such as cumbersome operation, unstable weighing results, accuracy and large hydrochloric acid consumption.
A device for batch determination of the moisture content of hydroxide-type anion exchange resin is designed. It adopts a basket structure and dynamic immersion exchange method, combined with a pH online monitor and a peristaltic pump automatic control system, to realize an automated transformation and drying process, reducing reagent consumption and weighing errors.
The stability and accuracy of the measurement results are improved, reagent consumption is reduced, weighing errors are eliminated, and batch transformation processing and water content measurement of anion exchange resin samples are realized.
Smart Images

Figure CN119861004A_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 water content of ion exchange resin refers to the internal water content contained in the resin particles after removing the external free water. It is one of the important properties of resin products. The water content of ion exchange resin is related to factors such as the type, structure, acidity and alkalinity, degree of crosslinking, exchange capacity, and ion form of the resin. If the resin chain breaks, the pore structure changes, and the exchange capacity decreases during use, its water content will also change accordingly. Therefore, the change in the water content of ion exchange resin can also reflect the change in its internal performance.
[0003] The conventional method for determining the water content of ion exchange resins is to remove the external 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, and finally calculate the water content by the change in mass. However, for hydroxyl type anion exchange resins, the strong base groups are prone to thermal degradation at high temperatures above 80°C, so the water content cannot be determined by the direct drying method.
[0004] The currently disclosed method for determining the water content of the hydroxyl type anion exchange resin is to use GB / T 5759-2000 "Determination of the water content of the oxy-type anion exchange resin" for testing. The prepared hydroxyl type anion exchange resin sample is accurately weighed and placed in a water content measuring device with constant weight. The water content measuring device is a small glass chromatography column. A quantitative amount of hydrochloric acid is passed through the ion exchange resin layer to completely transform the sample into the chlorine type. After washing with anhydrous ethanol to remove excess hydrochloric acid, the water content measuring device and the resin sample are placed in an oven at (105±3)°C for drying. The dry basis mass of the chlorine type is measured, and the mass increment generated during the transformation process is subtracted to calculate the dry basis mass of the hydroxyl type sample, and finally the water content is calculated. This method can effectively solve the problem of determining the water content of hydroxyl type anion exchange resin, but it also has the following disadvantages: first, it relies on manual operation, the process is cumbersome and labor-intensive; second, it is difficult to transfer all the ion exchange resins from the water content meter after transformation, so the two times before and after are placed on the electronic balance for weighing together with the water content meter. The length of the water content meter exceeds the common electronic balance weighing pan, and the shape is uneven. It is greatly affected by the placement position during weighing, which can easily cause unstable weighing results; third, there is a space between the lower part of the sand core and the piston of the water content meter, where liquid is easy to accumulate. If the accumulated liquid is not completely evaporated during the oven drying process, it will seriously affect the accuracy of the measurement results; fourth, in order to ensure complete transformation, a single ion exchange resin sample of about 1 g needs to be transformed with 200 mL~250 mL of hydrochloric acid, which consumes a large amount of reagents. Summary of the invention
[0005] In view of the problems existing in the prior art, the present invention provides a device and method for batch determination of the water content of hydroxyl type anion exchange resins, so as to solve the problems of the traditional chromatography column type water content determination device, which is complicated in process, easily causes unstable weighing results, high accuracy and large hydrochloric acid consumption. The device has a high degree of automation and is easy to operate. The anion exchange resin samples can be transformed in batches, the reagent consumption is reduced, the weighing error is eliminated, and the result stability and accuracy are better.
[0006] The present invention is achieved through the following technical solutions.
[0007] A device for batch determination of water content of hydroxyl type anion exchange resin, comprising a transformation reaction tank, an inlet peristaltic pump, an outlet peristaltic pump and a pH online monitor; A plurality of mesh baskets are placed in the transformation reaction tank, each mesh basket being used to place the hydroxide type anion exchange resin to be measured; One side of the transformation reaction tank is connected to a liquid storage tank through the end of an inlet pipeline, and an inlet peristaltic pump is installed on the inlet pipeline; The other side of the transformation reaction tank is connected to a waste liquid recovery tank through the end of the 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.
[0008] Preferably, the notch of the transformation reaction tank is provided with a top cover, the mesh basket is a cylindrical structure with a convex structure on the top, a plurality of circular holes are opened in the top cover, and the diameter of the circular holes is larger than the diameter of the cylinder wall of the mesh basket and smaller than the diameter of the top convexity of the mesh basket.
[0009] Preferably, the bottom and the wall of the mesh basket are provided with through holes, and the through holes can prevent the hydroxide-type anion exchange resin to be measured from leaking out of the mesh basket.
[0010] A method for batch determination of the water content of a hydroxyl anion exchange resin, based on the test device for the water content of a hydroxyl anion exchange resin described in any one of the above, comprises the following steps: S1, placing a number of baskets filled with hydrogen-oxygen type anion exchange resins to be determined in a transformation reaction tank, closing the outlet peristaltic pump, and opening the inlet peristaltic pump to flow hydrochloric acid into the transformation reaction tank. When the liquid level exceeds the anion exchange resin in the basket, the outlet peristaltic pump is opened, and the flow rates of the inlet peristaltic pump and the outlet peristaltic pump are adjusted to be consistent. 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; S2, observe the reading of the pH online monitor, and when the anion exchange resin has been converted into the chloride type, close the inlet peristaltic pump to discharge the remaining hydrochloric acid in the transformation reaction tank; S3, close the outlet peristaltic pump, open the inlet peristaltic pump to connect anhydrous ethanol to the transformation reaction tank, and open the outlet peristaltic pump when the liquid level exceeds the anion exchange resin in the net basket. The outflow liquid flows out to the waste liquid recovery tank through the outlet pipeline, the outlet peristaltic pump and the pH online monitor. When the pH is 7, stop, and take out all the net baskets for drying; S4, calculating the water content of the hydroxyl type anion exchange resin to be measured in each basket according to the mass of each basket in S1, the initial total mass of each basket filled with 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 wet basis strong base group capacity of the anion exchange resin in each basket. Preferably, in S1, when the liquid level exceeds the anion exchange resin in the basket by 1 cm to 2 cm, the outlet peristaltic pump is turned on.
[0011] 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.
[0012] Preferably, the concentration of the hydrochloric acid in S1 is 1 mol / L to 2 mol / L.
[0013] Preferably, in S2, when the pH value of the pH online monitor rises and then drops to a constant value, after continuously introducing hydrochloric acid for 10 min to 15 min, the anion exchange resin has been converted into the chloride type.
[0014] 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.
[0015] Preferably, S4 calculates the water content of the hydroxide-type anion exchange resin to be measured in each basket according to the following formula: ; X - the water content of the corresponding hydroxyl anion exchange resin to be determined in each basket in S1, expressed as a percentage; m 1—the mass of each basket in S1, in g; m 2—the total mass of each basket containing the anion exchange resin in S1, in g; m 3—The total mass of each basket containing the dried anion exchange resin in S3, in g; E 1—the wet basis total exchange capacity of the corresponding hydroxide anion exchange resin in each basket in S1, in mmol / g; E 2—Wet base capacity of the corresponding anion exchange resin in the hydroxide form in each basket of S1, in mmol / g.
[0016] Compared with the prior art, the present invention has the following beneficial technical effects: The present invention discloses a device for batch determination of water content of hydroxyl anion exchange resins. The device adopts a mesh basket structure design and has the characteristics of simple structure and small volume. The hydroxyl anion exchange resin sample to be determined can be directly placed therein and weighed on the weighing plate of a balance, thereby overcoming the problem of unstable weighing results of traditional water content measuring devices, avoiding weighing errors, and making the determination results more accurate. Before the transformation process of the hydroxyl anion exchange resin sample, multiple mesh baskets can be inserted into the transformation reaction tank. During the transformation process, the through holes on the mesh baskets allow the solution in the reaction tank to enter and contact and react with the sample, and the sample particles do not leak out. After the transformation reaction is completed, the excess acid is washed away with anhydrous ethanol, and then placed in an oven for drying, completing the main steps of weighing, batch exchange transformation and drying. During the transformation reaction process, the acidity of the effluent is measured by a pH online monitor. When the pH value is stable and unchanged, it can be judged that the reaction is complete, the hydroxyl anion exchange resin sample has been completely converted into the chloride type, and the introduction of hydrochloric acid is stopped, saving reagent consumption. The peristaltic pump automatically inputs and outputs the reaction solution. Compared with the traditional method of adding the solution with 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 ion exchange resin sample is maintained, so that the equilibrium reaction can continue to proceed in a positive direction. The device has a high degree of automation and is easy to operate. Compared with traditional devices, it consumes less reagents and eliminates weighing errors. The results are more stable and accurate, and the batch transformation of anion exchange resin samples is realized, thereby determining the water content.
[0017] The present invention discloses a method for batch determination of water content of hydroxyl type anion exchange resin. The ion exchange resin sample can be placed in a mesh basket with through holes for weighing, transformation reaction and drying. In the transformation process, a dynamic immersion exchange method is adopted. Hydrochloric acid or anhydrous ethanol is injected into the transformation reaction tank through an inlet peristaltic pump via an inlet pipeline. The transformation and water washing process can be accurately and quickly judged by a pH online monitor. The outflowing liquid is injected into a recovery tank via an outlet peristaltic pump via an outlet pipeline and a pH online monitor. The peristaltic pump automatically inputs and outputs the reaction solution. Compared with the traditional method of adding the solution by 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. 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 be continuously carried out in a positive direction. After the hydroxyl type anion exchange resin is converted into a chloride type, anhydrous ethanol is added to wash away the excess acid, thereby ensuring the accuracy of the measurement result. The use of a mesh basket for pre- and post-weighing and drying ensures the consistency of the determination 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 type anion exchange resin to be determined in each mesh basket in batches. In summary, compared with the traditional method, the method of the present invention has a higher degree of automation, less reagent consumption, and higher experimental efficiency, avoiding the problem of unstable weighing results caused by the large size and irregular shape of the traditional water content measuring device, and also has the advantages of rigorous process, controllable conditions, and accurate and reliable results. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 It is a schematic diagram of the device for batch determination of water content of hydroxyl type anion exchange resin according to the present invention.
[0019] Figure 2 for Figure 1 Partial cross-sectional view of the middle basket.
[0020] Figure 3 for Figure 1 Schematic diagram of the structure of the middle net basket.
[0021] 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
[0022] 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 embodiments and drawings, which are intended to explain the present invention rather than to limit it.
[0023] 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 transformation reaction tank 1 through the top cover 2, and the hydroxide type anion exchange resin to be measured is placed in the mesh basket 3. The transformation 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 transformation reaction tank 1. The top cover 2 is plugged into the notch of the transformation reaction tank 1 and the upper surfaces of the two are flush, so the top cover 2 is detachable, and the mesh basket 3 is a cylindrical structure. A plurality of circular holes are opened in the top cover 2, so that the mesh basket 3 can be vertically placed in the transformation reaction tank 1 through the corresponding holes, and the top protrusion is hung on the top cover 2.
[0024] A liquid inlet 4 is provided on one side of the upper outer wall of the transformation reaction tank 1. The inlet peristaltic pump 6 is connected to the liquid inlet 4 through 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 be filled with 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 through 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.
[0025] The height of the transformation reaction tank 1 is 5 cm to 10 cm, and the material is polymethyl methacrylate or glass or other acid-resistant materials. 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, so that the net basket 3 can be inserted into the transformation reaction tank 1 from the hole in the top cover 2 without falling in, and the bottom of the raised structure is flush with the upper surface of the notch of the transformation reaction tank 1.
[0026] The net basket 3 is in a mesh shape or is covered with strip-shaped through holes. The specific through hole structure design of the net basket 3 can be as follows: Figure 2 As shown, through holes are provided at the bottom and the wall of the cylinder, so that the liquid can quickly enter and exit the basket. The through holes are evenly distributed in the shape of strips, with a length of 1 mm to 2 mm and a width of 0.10 mm to 0.20 mm, which is smaller than the diameter of the ion exchange resin, so that the solution in the transformation reaction tank 1 can contact the sample inside the basket 3, and can prevent the hydroxide type anion exchange resin to be measured from leaking from 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. The raised part is provided with an arc handle for easy picking, and the material is resistant to high temperature and acid corrosion, such as polytetrafluoroethylene or phenolic resin.
[0027] The present invention provides a method for batch determination of water content of hydroxide type anion exchange resin, based on the above-mentioned testing device, comprising the following steps: In the first step, all the baskets 3 were cleaned and dried in an oven at (105±3)℃ to constant weight. m 1; In the second step, the free water outside the hydroxyl type anion exchange resin sample to be tested is removed by centrifugation. 2 g to 4 g of the ion exchange resin sample is weighed with an electronic balance and placed in the mesh basket 3 which has been weighed constant in the first step. The total mass of the sample and the mesh basket 3 is read. m 2; The third step is to place the net basket 3 containing the hydroxyl type anion exchange resin sample into the transformation reaction tank 1 through the top cover 2, and the top protrusion is suspended on the top cover 2, close the outlet peristaltic pump 9, connect the inlet pipe 5 to 1 mol / L~2 mol / L hydrochloric acid, and use the inlet peristaltic pump 6 to let the hydrochloric acid flow into the transformation reaction tank 1 through the liquid inlet 4. When the liquid level exceeds the ion exchange resin layer in the net 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), start the outlet peristaltic pump 9, and adjust the flow rates of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 to be consistent, which is 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; 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 min to 15 min to ensure that the transformation reaction is complete. Turn off the inlet peristaltic pump 6 to discharge the remaining hydrochloric acid in the transformation reaction tank 1. At this time, the hydroxide type anion exchange resin sample has been converted into the chloride type. The fifth step is to close the outlet peristaltic pump 9, connect the inlet pipe 5 to the 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~2 cm, 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, which is 8 mL / min~16 mL / min. The outlet outflow solution flows into the waste liquid recovery tank 11. When the pH of the outlet outflow solution is 7, it stops. At this time, the excess hydrochloric acid in the anion exchange resin is washed away, and the outflow solution is neutral; Step 6: Take out the net basket 3 containing the anion exchange resin sample, place it in a tray and put it into a preheated constant temperature drying oven, and dry it at (105±3)℃ for 2 hours; Step 7: After drying, place the basket 3 containing the anion exchange resin sample in a dryer, cool it to room temperature, and weigh the mass after drying. m 3; Step 8: Determine the wet basis total exchange capacity of the anion exchange resin according to GB / T5760 "Method for 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; In the ninth step, the water content of the hydroxide type anion exchange resin is calculated according to the following formula (1).
[0028] (1) in: X — moisture content, expressed as a percentage; m 1—the mass of the basket in the first step, in g; m 2—Total mass of the ion exchange resin sample and basket in the second step, in grams; m 3—Total mass of the ion exchange resin sample and the basket after drying in step 7, in g; E 1—Wet basis total exchange capacity of anion exchange resin, in mmol / g; E 2—Wet base capacity of anion exchange resin, expressed in mmol / g.
[0029] Example 1 The present invention provides a method for batch determination of water content of hydroxide type anion exchange resin, which specifically comprises the following steps: In the first step, the eight baskets 3 were cleaned and numbered, and then dried in an oven at 105°C to constant weight. The mass of each basket was weighed, which were m 1i , i=1~8; In the second step, the free water outside 8 portions of unused hydroxyl anion exchange resins were removed by centrifugation. 3.0-3.1 g of ion exchange resin samples were weighed using an electronic balance and placed in the net basket 3 weighed in the first step. The total mass of the ion exchange resin sample and the net basket 3 was read. m 2i , i=1~8; The third step is to insert 8 baskets 3 containing hydroxyl type anion exchange resin samples into the transformation reaction tank 1 through the top cover 2, close the outlet peristaltic pump 9, connect the inlet pipe 5 to 1 mol / L hydrochloric acid, and use the inlet peristaltic pump 6 to let the hydrochloric acid 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, and adjust the flow rate of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 to be consistent, which is 15 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; 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 min and close 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 hydroxyl type anion exchange resin sample has been converted into the chloride type. Step 5: close the outlet peristaltic pump 9, connect the inlet pipe 5 to the 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, and adjust the flow rates of the inlet peristaltic pump 6 and the outlet peristaltic pump 9 to be consistent, which is 12 mL / min. The outlet outflow solution flows into the waste liquid recovery tank 11. When the outlet outflow solution is neutral, stop, and the excess hydrochloric acid in the anion exchange resin is washed away. 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)℃ for 2 hours; Step 7: After drying, place the eight baskets 3 containing the anion exchange resin samples in a dryer, cool to room temperature, and weigh the mass after drying. m 3i , i=1~8; Step 8: Determine the wet basis total exchange capacity of the anion exchange resin according to GB / T5760 "Method for 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; The ninth step is to calculate the water content of 8 hydroxide-type anion exchange resins. The results are shown in Table 1.
[0030] Table 1 Water content determination data
[0031] The water content of unused hydroxyl anion exchange resin samples is generally 50%~60%, and the water content of the resin samples in Table 1 is 50%~60%, indicating that the determination results are reasonable. The water content of the eight samples in the first step was determined using the current standard method GB / T 5759-2000 "Determination of water content of oxy-anion exchange resin" and compared with the water content results in Table 1. The absolute difference between the determination results of the two methods is 0.1%~1.0%, indicating that the determination results of this method are accurate.
Claims
1. A device for batch determination of water content of hydroxide-type anion exchange resin, characterized in that: It comprises 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 an outlet pipeline (8), an outlet peristaltic pump (9) and a pH online monitor (10) are installed on the outlet pipeline (8), and the pH online monitor (10) is arranged close to the waste liquid recovery tank (11).
2. The device 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 net basket (3) is a cylindrical structure with a convex structure on the top; 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 net basket (3) and smaller than the diameter of the top convex of the net basket (3).
3. The device 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 hydroxide-type anion exchange resin to be measured from leaking out of the mesh basket (3).
4. A method for batch determination of water content of hydroxide anion exchange resin, characterized in that: The testing device for the water content of the hydroxide type anion exchange resin according to any one of claims 1 to 3 comprises the following steps: S1, placing a plurality of baskets (3) containing the hydroxyl type anion exchange resin to be determined 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), and opening the outlet peristaltic pump (9) when the liquid level exceeds the anion exchange resin in the basket (3), while 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) through the outlet pipeline (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), start the inlet peristaltic pump (6) to connect anhydrous ethanol to the transformation reaction tank (1), and start the outlet peristaltic pump (9) when the liquid level exceeds the anion exchange resin in the net basket (3). The outflow liquid flows through the outlet pipeline (8), the outlet peristaltic pump (9) and the pH online monitor (10) to the waste liquid recovery tank (11). When the pH is 7, stop, and take out all the net baskets (3) for drying; S4, calculating the water content of the hydroxyl type anion exchange resin to be measured in each basket (3) according to 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).
5. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 4, 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.
6. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 4, 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~20 mL / min.
7. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 4, characterized in that: The concentration of hydrochloric acid in S1 is 1 mol / L~2 mol / L.
8. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 7, characterized in that: In S2, when the pH value of the pH online monitor (10) rises and then drops to a constant value, after continuously introducing hydrochloric acid for 10 min to 15 min, the anion exchange resin has been converted into the chloride type.
9. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 4, 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 at the same time, 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.
10. The method for batch determination of water content of hydroxide-type anion exchange resin according to claim 4, characterized in that: S4 calculates the water content of the hydroxyl type 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—the 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 hydroxide-type anion exchange resin in each basket (3) in S1, in mmol / g; E 2—Wet base group capacity of the corresponding anion exchange resin in the hydroxide form in each basket (3) in S1, in mmol / g.
Citation Information
Patent Citations
Method for removing phosphorus and boron from silicon dioxide mine
CN101445246A
Automatic neutralizing chemical feeding device and method for hydrochloric acid regeneration and desiliconization
CN103011080A
Apparatus for determining maximum strong group regeneration capacity of oxyhydrogen anion exchange resin
CN105277543A
An ion exchange resin vacuum drying test method and device
CN107044945A
Device and method for testing temperature resistance of anion exchange resin
CN116735648A