CN113295761B - Dynamic adsorption experimental device for cesium ion removal - Google Patents
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Abstract
The invention relates to a dynamic adsorption experimental device for cesium ion removal, and belongs to the technical field of dynamic adsorption devices. The device comprisesPump, the feed liquor valve, the drain valve, N I type adsorption column, the sensor, collection control system and display screen, the inlet end of N I type adsorption column, the outlet end corresponds parallelly connected on inlet main line, outlet main line, the inlet end of every I type adsorption column, the inlet valve is installed to the outlet end corresponds, the drain valve, and install the sensor between inlet valve and the drain valve, install the pump on the inlet main line that is close to the inlet end, sensor and display screen all are connected with collection control system, collection control system is connected with outside computer, the device can be used for evaluating different adsorption materials and to Cs under different conditions + Is used for the adsorption capacity of the catalyst; the II-type adsorption column is arranged on the liquid inlet main pipeline between the pump and the I-type adsorption column, so that the interference Cs can be removed preferentially + Other impurities adsorbed.
Description
Technical Field
The invention relates to a dynamic adsorption experimental device for cesium ion removal, and belongs to the technical field of dynamic adsorption devices.
Background
In industrial production, a large amount of sewage containing harmful elements is discharged, and the treatment of certain specific elements requires a large amount of resources. The dynamic adsorption device dynamically adsorbs impurities in the sewage, so that the aim of adsorbing harmful elements in the sewage is fulfilled. At present, the existing adsorption device is difficult to collect impurities in sewage, is inconvenient for workers to detect the sewage, can not effectively adsorb harmful elements in the sewage, and especially can not achieve a good effect on cesium ion adsorption. The existing adsorption device cannot preferentially remove other organic or inorganic impurities interfering with adsorption when cesium ions are adsorbed, has a complex structure and complex operation, cannot reflect and control the experimental process in real time, has single adsorption material filled in the device, and cannot perform investigation and comparison of various adsorption materials at the same time.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a dynamic adsorption experimental device for cesium ion removal, which can be used for evaluating the adsorption capacity of different adsorption materials on cesium ions under different conditions (such as parameters of flow rate, temperature, pressure, pH and the like) under the cooperation of inductively coupled plasma mass spectrometry (ICP-MS) equipment, can realize effective adsorption of cesium ions in solution, and has simple structure and easy operation.
The aim of the invention is achieved by the following technical scheme.
A dynamic adsorption experimental device for cesium ion removal comprises a pump, a liquid inlet valve, a liquid outlet valve, N I-type adsorption columns, a sensor, an acquisition control system and a display screen; wherein, N is a positive integer, and the type of the sensor is selected according to actual needs (such as a sensor for measuring parameters of flow, temperature, pressure, pH and the like can be selected);
the inlet end of N I type adsorption columns is parallelly connected on inlet main pipeline, and the liquid outlet end of N I type adsorption columns is parallelly connected on outlet main pipeline, and the inlet valve is installed to the inlet end of every I type adsorption column, and the liquid outlet valve is installed to the liquid outlet end of every I type adsorption column, installs the sensor between the inlet valve of every I type adsorption column and the liquid outlet valve, installs the pump on inlet main pipeline that is close to the inlet end, and sensor and display screen all are connected with collection control system, and collection control system is connected with outside computer.
The type I adsorption column is filled with an adsorption material having an adsorption effect on cesium ions, such as cation exchange resin, alumina, graphene-based adsorbent, humic acid-based resin, zeolite, coal-based adsorbent prepared from lignite, long flame coal, anthracite, etc.
Further, the graphene-based adsorbent is preferably a GO/CS/KCuHCF composite aerogel composed of Graphene Oxide (GO), chitosan (CS) and potassium ferrocyanide (KCuHCF), and is specifically prepared by the following method: mixing GO dispersion with CS dispersion with deacetylation degree not less than 80%, shaking to colloid, standing and removing uncrosslinked reactant, and drying to obtain gel product with Cu (NO 3 ) 2 Leaching the solution to make Cu 2+ The reaction with oxygen-containing and nitrogen-containing functional groups of the composite gel until the effluent is blue, then washing with water until the effluent is colorless, and leaching with potassium ferrocyanide solution to make the potassium ferrocyanide react with Cu 2+ Loading KCuHCF on the gel until the effluent is light yellow, and finally washing with water until the effluent is colorless to obtain the once-loaded GO/CS/KCuHCF composite aerogel;
the once-loaded GO/CS/KCuHCF composite aerogel is dried to near dryness (i.e. NO obvious wet stain on the surface), cu (NO 3 ) 2 Leaching the solution to make Cu 2+ The reaction with oxygen-containing and nitrogen-containing functional groups of the composite gel until the effluent is blue, then washing with water until the effluent is colorless, and leaching with potassium ferrocyanide solution to make the potassium ferrocyanide react with Cu 2+ Loading KCuHCF on the gel until the effluent is light yellow, and finally washing with water until the effluent is colorless to obtain the secondarily loaded GO/CS/KCuHCF composite aerogel;
the secondary loaded GO/CS/KCuHCF composite aerogel is dried near (i.e. dried until the surface has NO obvious wet stain), cu (NO 3 ) 2 Leaching the solution to make Cu 2+ The reaction with oxygen-containing and nitrogen-containing functional groups of the composite gel until the effluent is blue, then washing with water until the effluent is colorless, and leaching with potassium ferrocyanide solution to make the potassium ferrocyanide react with Cu 2+ Loading KCuHCF on the gel until the effluent is light yellow, and finally washing with water until the effluent is colorless to obtain the GO/CS/KCuHCF composite aerogel loaded for three times;
the primary loaded GO/CS/KCuHCF composite aerogel, the secondary loaded GO/CS/KCuHCF composite aerogel and the tertiary loaded GO/CS/KCuHCF composite aerogel can be used as graphene adsorbents for removing radioactive cesium ions in water;
further, the concentration of the GO dispersion liquid is 2 mg/mL-10 mg/mL, preferably 7 mg/mL-8 mg/mL; the concentration of the CS dispersion is 1 mg/mL-10 mg/mL, preferably 8 mg/mL-10 mg/mL; the volume ratio of GO dispersion liquid to CS dispersion liquid is (5-15): 1, preferably (9 to 10): 1, a step of;
further, the mass ratio of CS in the CS dispersion to GO in the GO dispersion is preferably (9-27): 100;
further, acetic acid is usually selected as a medium of the CS dispersion liquid, and the volume fraction of the acetic acid in the CS dispersion liquid is preferably 1% -3.5%;
further, it is preferable to remove the uncrosslinked reactant after standing for 12 to 48 hours;
further, cu (NO 3 ) 2 The concentration of the solution is 0.01M-0.10M, preferably 0.05M-0.06M; the concentration of the potassium ferrocyanide solution is 0.01M-0.10M, preferably 0.05M-0.06M; cu (Cu) 2+ The molar ratio of the potassium ferrocyanide to the potassium ferrocyanide is 2:1-1:2, preferably (0.8-1.2): 1.
Further, the device also comprises a type II adsorption column, wherein activated carbon, bentonite, an X-type molecular sieve or a Y-type molecular sieve is filled in the type II adsorption column;
the liquid inlet valve is arranged at the liquid outlet end of the II type adsorption column, and the sensor is arranged between the liquid inlet valve and the liquid outlet valve.
Further, the materials of the type I adsorption column and the type II adsorption column are organic glass.
Further, the aspect ratio of the type I adsorption column and the type II adsorption column is preferably 10 to 15.
The device can test the adsorption efficiency of different adsorption materials at different flow rates, automatically detect the flow, temperature, pressure, pH and other parameters of each test point, and judge the adsorption capacity of different adsorption materials on cesium ions by combining ICP equipment. In order to facilitate sampling and detection, an evacuation valve and a liquid outlet are arranged behind the liquid outlet valve of each I-type adsorption column; an evacuation valve and a liquid outlet are arranged in front of the liquid inlet valve of the II-type adsorption column.
The beneficial effects are that:
the device can be used for evaluating the adsorption capacity of different adsorption materials on cesium ions under different conditions (such as parameters of flow rate, temperature, pressure, pH and the like), and can preferentially remove other impurities interfering with cesium ion adsorption, and especially, the effective adsorption of cesium ions in solution can be realized by selecting a proper adsorption material; the data monitored by the on-line sensor can reflect the experimental process in real time, and transparent organic glass is adopted, so that experimental research and display are facilitated.
Drawings
Fig. 1 is a schematic structural diagram of a dynamic adsorption experimental apparatus for cesium ion removal in an embodiment.
Fig. 2 is a three-dimensional schematic diagram of a dynamic adsorption experimental apparatus for cesium ion removal in the example.
FIG. 3 shows Cs in the examples + Removal rate graph of low-level wastewater on dynamic adsorption device for cesium ion removal.
Wherein, the P-101-pump, the T-101-II type adsorption column, the T-102-T-105-I type adsorption column, the 1-5-liquid inlet valve, the 7-11-liquid outlet valve, the 6, the 12-15-evacuation valve, the 16-pH sensor, the 17-liquid inlet main pipeline, the 18-liquid outlet main pipeline, the TI-101-TI-105-temperature sensor, the PI-101-PI-105-pressure sensor, the FI-101-FI-105-flow sensor and the AP-101-AP-105-liquid outlet.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and detailed description, wherein the process is a conventional process unless otherwise specified, and wherein the starting materials are commercially available from the public sources. In addition, in the description of the present invention, it should be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present invention.
The dynamic adsorption experimental device for cesium ion removal in the following embodiment comprises a pump P-101, five liquid inlet valves 1-5, five liquid outlet valves 7-11, four I-type adsorption columns T-102-T-105, II-type adsorption column T-101, five temperature sensors TI-101-TI-105, five flow sensors FI-101-FI-105, five pressure sensors PI-101-PI-105, a pH sensor 16, an acquisition control system and a display screen, as shown in fig. 1 and 2;
the pump P-101 is an electromagnetic diaphragm pump with the highest pressure of 0.5MPa and the flow rate of more than 10L/h;
the four I-type adsorption columns T-102 to T-105 are made of organic glass, and the four I-type adsorption columns T-102 to T-105 are sequentially filled with silicon dioxide pellets (with the particle size of 30 to 100 meshes), cation exchange resin (002 CR, the hydrogen ion exchange capacity of 5.0 to 5.2 mmol/g), spherical alumina (with the diameter of 1 to 2 mm) and GO/CS/KCuHCF composite aerogel;
the material of the II-type adsorption column T-101 is organic glass, and activated carbon is filled in the II-type adsorption column T-101;
the liquid inlet ends of the four I-type adsorption columns T-102-T-105 are connected in parallel on the liquid inlet main pipeline 17, the liquid outlet ends of the four I-type adsorption columns T-102-T-105 are connected in parallel on the liquid outlet main pipeline 18, the liquid inlet ends of the four I-type adsorption columns T-102-T-105 are provided with four liquid inlet valves 2-5 in a one-to-one correspondence in sequence, the liquid outlet ends of the four I-type adsorption columns T-102-T-105 are provided with four liquid outlet valves 8-11 in a one-to-one correspondence in sequence, flow sensors FI-102-FI-105, temperature sensors TI-102-TI-105 and pressure sensors PI-102-PI-105 are respectively arranged between the liquid inlet valves and the liquid outlet valves corresponding to the four I-type adsorption columns T-102-T-105, and the liquid outlet valves corresponding to each other are provided with evacuation valves 12-15 and liquid outlet ports AP-102-AP-105 in a one-to-one correspondence in sequence; a pump P-101 is arranged on the liquid inlet main pipeline 17 close to the liquid inlet end, a II-type adsorption column T-101 is arranged on the liquid inlet main pipeline 17 between the pump P-101 and four I-type adsorption columns T-102-T-105, a liquid inlet valve 1 is arranged at the liquid inlet end of the II-type adsorption column T-101, a liquid outlet valve 7 is arranged at the liquid outlet end of the II-type adsorption column T-101, a flow sensor FI-101, a temperature sensor TI-101 and a pressure sensor PI-101 are arranged between the liquid inlet valve 1 and the liquid outlet valve 7, and an exhaust valve 6 and a liquid outlet AP-101 are arranged between the pump P-101 and the liquid inlet valve 1; the pH sensor 16, five flow sensors FI-101 to FI-105, five temperature sensors TI-101 to TI-105, five pressure sensors PI-101 to PI-105, the pH sensor 16 and a display screen are all connected with the acquisition control system, and the acquisition control system is connected with an external computer.
The specific preparation steps of the GO/CS/KCuHCF composite aerogel are as follows:
(1) Mixing 2.5mL of GO dispersion with concentration of 8.0mg/mL and 0.25mL of CS with concentration of 8.0mg/mL (deacetylation degree (D.D): 80% -95%, volume fraction of 2.5% acetic acid medium) and vortex oscillating for 10s to form gel, transferring to 5mL syringe (bottom is filled with 200 mesh nylon filter screen 2 layers), standing for 24h, adding water to wash gel to remove uncrosslinked CS, and after the gel product is nearly dry, adopting Cu (NO) with concentration of 0.06M 3 ) 2 Eluting the solution until the effluent is blue, washing with water until the effluent is colorless, eluting the solution until the effluent is pale yellow with 0.05M potassium ferrocyanide solution, and washing with water until the effluent is colorless to obtain the GO/CS/KCuHCF composite aerogel loaded once;
(2) The once loaded GO/CS/KCuHCF composite aerogel is near-dry, cu (NO) with concentration of 0.06M is adopted first 3 ) 2 Eluting the solution until the effluent is blue, washing with water until the effluent is colorless, eluting the solution until the effluent is pale yellow with 0.05M potassium ferrocyanide solution, and washing with water until the effluent is colorless to obtain the secondarily loaded GO/CS/KCuHCF composite aerogel;
(3) The GO/CS/KCuHCF composite aerogel loaded for the second time is nearly dried, the leaching operation of the step (3) is repeated to obtain the GO/CS/KCuHCF composite aerogel loaded for the third time, and the GO/CS/KCuHCF composite aerogel is obtained;
the prepared 4mg GO/CS/KCuHCF composite aerogel was added as an adsorption material to 10mL of the mixture containing pH 5.Cesium ion solution of 7 (Cs + 155.9 mg/L), magnetically stirring at 25deg.C for 3 hr, performing solid-liquid separation, and measuring Cs with inductively coupled plasma mass spectrometer (ICP-MS) + Cs before adsorption in solution + Concentration C of (2) 0 =155.9 mg/L and Cs after adsorption + Concentration C e =110.0mg/L, calculated saturated adsorption capacity Q under test conditions e ＝114.8mg/g。
Example 1
In a dynamic adsorption experimental device for cesium ion removal, the inner diameters of a type II adsorption column T-101 and four type I adsorption columns T-102-T-105 are 28mm, the lengths are 350mm and the wall thicknesses are 4mm, and CsNO is treated by adopting the device 3 Aqueous solution (from 194.8mg CsNO) 3 And 20L deionized water) is specifically prepared as follows:
the liquid inlet of the liquid inlet main pipeline 17 is connected with CsNO 3 In a 25L bucket of the aqueous solution, a liquid inlet valve 1 and a liquid outlet valve 7 of a II-type adsorption column T-101 are opened, a liquid inlet valve 2 and a liquid outlet valve 8 of a silicon dioxide pellet I-type adsorption column T-102 are opened (liquid inlet valves 3-5 and liquid outlet valves 9-11 of other three I-type adsorption columns T-103-T-105 are closed), and the output frequency of a pump P-101 is set to be 24H; turning on a switch of the pump P-101, simultaneously turning on a stopwatch to start timing, sampling a sample with 5mL centrifuge tubes every 5min, marking the sampled 5mL centrifuge tubes as C1, C2, C3 and C4 … … C24 in sequence, and sealing the sampled sample tubes with sealing films for ICP test; opening a liquid inlet valve 3 and a liquid outlet valve 9 of a type I adsorption column T-103 filled with 002CR cation exchange resin, closing a liquid inlet valve 2 and a liquid outlet valve 8 of a type I adsorption column T-102 filled with silica pellets, simultaneously starting a stopwatch, timing, taking a sample with a 5mL centrifuge tube every 5min, marking the sampled 5mL centrifuge tube as S1, S2, S3 and S4 … … S24 in sequence, and sealing the sampled sample tube with a sealing film for ICP test; opening a liquid inlet valve 4 and a liquid outlet valve 10 of a spherical alumina I-type adsorption column T-104, closing a liquid inlet valve 3 and a liquid outlet valve 9 of a 002CR cation exchange resin I-type adsorption column T-103, simultaneously opening a stopwatch to start timing, taking a sample with 5mL centrifuge tubes every 5min, and marking the sampled 5mL centrifuge tubes in sequenceSealing the sampled sample tubes with sealing films for Q1, Q2, Q3 and Q4 … … Q24 for ICP test; opening a liquid inlet valve 5 and a liquid outlet valve 11 of a GO/CS/KCuHCF composite aerogel I type adsorption column T-105, closing a liquid inlet valve 4 and a liquid outlet valve 10 of a spherical alumina I type adsorption column T-104, simultaneously starting a stopwatch, timing, taking a sample every 5min by using a 5mL centrifuge tube, marking the sampled 5mL centrifuge tube as F1, F2, F3 and F4 … … F24 in sequence, and sealing the sampled sample by using a sealing film for ICP test; and closing the switch of the pump P-101, stopping timing, closing the liquid inlet valve 5 and the liquid outlet valve 11 of the I-type adsorption column T-105 filled with the GO/CS/KCuHCF composite aerogel, and closing the liquid inlet valve 1 and the liquid outlet valve 7 of the II-type adsorption column T-101.
In the testing process, the maximum flow rate of the inlet of the liquid inlet main pipeline 17 can reach 0.3L/min, and the maximum flow rate of the outlets of the four I-type adsorption columns T-102-T-105 can reach 0.1L/min; the average value of the inlet flow rate of the liquid inlet main pipeline 17 is 0.2L/min, namely 12L/h. As can be seen from FIG. 3, the GO/CS/KCuHCF composite aerogel can realize the removal rate of cesium ions of more than 99%, and the three separation columns of 002CR cation exchange resin, spherical alumina and silica pellets appear to have Cs at the feeding flow rate of 2.5L/h + Effectively retain, possibly of a single species with cesium ions, in the absence of Na + 、K + The plasma competes for ions and the initial concentration of cesium ions is higher and also directly related to the filler itself or the charge mass. In addition, it can be seen from fig. 3 that alumina has a relatively constant decay in cesium ion removal rate over time.
In summary, the above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A dynamic adsorption experimental apparatus for cesium ion is got rid of, its characterized in that: the device comprises a pump, a liquid inlet valve, a liquid outlet valve, N I-type adsorption columns, a sensor, an acquisition control system and a display screen; wherein N is a positive integer, and the I-type adsorption column is filled with an adsorption material with adsorption effect on cesium ions;
the liquid inlet ends of N I-type adsorption columns are connected in parallel on a liquid inlet main pipeline, the liquid outlet ends of N I-type adsorption columns are connected in parallel on a liquid outlet main pipeline, a liquid inlet valve is arranged at the liquid inlet end of each I-type adsorption column, a liquid outlet valve is arranged at the liquid outlet end of each I-type adsorption column, a sensor is arranged between the liquid inlet valve and the liquid outlet valve of each I-type adsorption column, a pump is arranged on the liquid inlet main pipeline close to the liquid inlet end, the sensor and a display screen are both connected with an acquisition control system, and the acquisition control system is connected with an external computer;
the adsorption material filled in the I-type adsorption column is a graphene adsorbent, the graphene adsorbent is GO/CS/KCuHCF composite aerogel composed of graphene oxide, chitosan and potassium ferrocyanide, and the GO/CS/KCuHCF composite aerogel is primary-loaded GO/CS/KCuHCF composite aerogel, secondary-loaded GO/CS/KCuHCF composite aerogel or tertiary-loaded GO/CS/KCuHCF composite aerogel prepared by adopting the following method:
mixing GO dispersion with CS dispersion with deacetylation degree not less than 80%, oscillating to colloid, standing and removing uncrosslinked reactant, and drying the colloid product with Cu (NO 3 ) 2 Eluting the solution until the effluent is blue, washing with water until the effluent is colorless, eluting with a potassium ferrocyanide solution until the effluent is pale yellow, and washing with water until the effluent is colorless to obtain once-loaded GO/CS/KCuHCF composite aerogel;
the once loaded GO/CS/KCuHCF composite aerogel is near-dry, cu (NO 3 ) 2 Eluting the solution until the effluent is blue, washing with water until the effluent is colorless, eluting with a potassium ferrocyanide solution until the effluent is pale yellow, and washing with water until the effluent is colorless to obtain a secondary-loaded GO/CS/KCuHCF composite aerogel;
the secondary loaded GO/CS/KCuHCF composite aerogel is near-dry, cu (NO 3 ) 2 Eluting with water until the effluent is blue, eluting with potassium ferrocyanide solution until the effluent is colorlessAnd finally, washing with water until the effluent is light yellow, and obtaining the GO/CS/KCuHCF composite aerogel loaded for three times.
2. The dynamic adsorption assay device for cesium ion removal of claim 1, wherein: the concentration of the GO dispersion liquid is 2 mg/mL-10 mg/mL, the concentration of the CS dispersion liquid is 1 mg/mL-10 mg/mL, and the volume ratio of the GO dispersion liquid to the CS dispersion liquid is (5-15): 1, a step of; acetic acid is selected as a medium of the CS dispersion liquid, and the volume fraction of the acetic acid in the CS dispersion liquid is 1% -3.5%; cu (NO) 3 ) 2 The concentration of the solution is 0.01M-0.10M, the concentration of the potassium ferrocyanide solution is 0.01M-0.10M, cu 2+ The molar ratio of the potassium ferrocyanide to the potassium ferrocyanide is 2:1-1:2.
3. The dynamic adsorption assay device for cesium ion removal of claim 2, wherein: the concentration of the GO dispersion liquid is 7 mg/mL-8 mg/mL, the concentration of the CS dispersion liquid is 8 mg/mL-10 mg/mL, and the volume ratio of the GO dispersion liquid to the CS dispersion liquid is (9-10): 1, a step of; cu (NO) 3 ) 2 The concentration of the solution is 0.05M-0.06M, the concentration of the potassium ferrocyanide solution is 0.05M-0.06M, cu 2+ The molar ratio of the potassium ferrocyanide to the potassium ferrocyanide is (0.8-1.2) 1.
4. The dynamic adsorption assay device for cesium ion removal of claim 1, wherein: and (3) standing for 12-48 hours, and removing the uncrosslinked reactant.
5. The dynamic adsorption assay device for cesium ion removal of claim 1, wherein: the device also comprises a type II adsorption column, wherein activated carbon, bentonite, an X-type molecular sieve or a Y-type molecular sieve is filled in the type II adsorption column;
the liquid inlet valve is arranged at the liquid outlet end of the II type adsorption column, and the sensor is arranged between the liquid inlet valve and the liquid outlet valve.
6. The dynamic adsorption assay device for cesium ion removal of claim 5, wherein: the materials of the type I adsorption column and the type II adsorption column are organic glass.
7. The dynamic adsorption assay device for cesium ion removal of claim 5, wherein: the length-diameter ratio of the type I adsorption column and the type II adsorption column is 10-15.
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