CN114471474B - Resin material capable of selectively adsorbing Am (III) in high acid environment and preparation method thereof - Google Patents
Resin material capable of selectively adsorbing Am (III) in high acid environment and preparation method thereof Download PDFInfo
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- CN114471474B CN114471474B CN202210131125.2A CN202210131125A CN114471474B CN 114471474 B CN114471474 B CN 114471474B CN 202210131125 A CN202210131125 A CN 202210131125A CN 114471474 B CN114471474 B CN 114471474B
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
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Abstract
The invention relates to a new application of a known material and a preparation method of a material prepared from the material, in particular to an adsorption Am (III) in a high-acid environment by using TODGA silicon-based resin and a method for preparing a resin material capable of selectively adsorbing Am (III) in the high-acid environment by using TODGA. The new application of the TODGA silicon-based resin is that the TODGA silicon-based resin is used for selectively adsorbing Am (III). More preferably, one of the materials of the present invention for selective adsorption Am (III) is to adsorb TODGA onto SiO2 particles. A related simulation test shows that the TODGA has a strong adsorption effect on Am-241 and other nuclides, has excellent high acid resistance, and is a very potential material which can be applied to the separation and enrichment of Am-241 in radioactive waste liquid by combining the TODGA and SiO2 to prepare the solid-phase resin.
Description
Technical Field
The invention relates to a new application of a known material and a preparation method of a material prepared from the material, in particular to an adsorption Am (III) in a high-acid environment by using TODGA silicon-based resin and a method for preparing a resin material capable of selectively adsorbing Am (III) in the high-acid environment by using TODGA.
Background
Alpha radionuclides represented by Am-241 in high level waste liquid are major contributors to long-term radioactivity, and present a great challenge to the supervision of high level waste liquid storage. The method can effectively separate the alpha radionuclide, greatly reduce the volume of the high-level waste liquid to be treated (see document (1) Song Chongli), the conceptual flow of the high-level waste liquid in China [ J ]. Atomic energy science and technology, 1995, 29 (3): 9. (2) [1] Zhao Haogui, and the research on the separation method of the high-level waste liquid based on the graphene oxide film [ D ]. University of Chinese academy of sciences), and facilitate the smooth proceeding of the subsequent transmutation treatment or glass solidification process. Therefore, the search for a means for effectively removing the alpha nuclides in the post-treatment of spent fuel remains a major topic at the present stage.
TODGA is an extractant with amide as a main functional group, and the application of TODGA at the present stage is separation and enrichment of lanthanoid and actinoid. ( See literature: (1) geist A, mullich U, magnusson D, et al actionide (III)/lanthanide (III) separation via selective aqueous complexation of actinides (III) using a hydrophilic 2, 6-bis (1, 2, 4-triazin-3-yl) -pyridine in nitric acid [ J ]. Solvent Extraction and ion exchange, 2012, 30 (5): 433-444 ] (2) Lumetta G J, gelis A V, carter J C, et al, the Actinide-lanthanide separation concept [ J ]. Solvent Extraction and Ion Exchange, 2014, 32 (4): 333-347 (3) Arginide D, battisti P, giardina I Extraction chromatography with DGA resin for The determination of americium and curium in biological samples by high resolution alpha spectrometry [ J ]. Journal of Radioanalytical and Nuclear Chemistry, 2016, 309 (1): 279-284. )
SiO is used in the prior art 2 There are generally two ways to combine with TODGA, the external method and the impregnation method. The external connection method uses aminosilane as coupling agent, and uses the coupling agent in SiO 2 Introducing amino groups thereon, followed by chlorination of the amino groups with acyl chloride DODGA reaction (see literature (1) He Y, huang Y, jin Y, et al Well-defined nanostructured surface-imprinted polymers for highly selective magnetic separation of fluoroquinolones in human urine [ J)]. ACS applied materials &Interface, 2014, 6 (12): 9634-9642 (2) Li Jingrui. N, N-dioctyl diglycolamine acid bonded solid phase Material preparation and separation rare earth Performance study [ D ]]University of Beijing technology 2021 (3) Liu D, li Y, deng J, et al Synthesis and characterization of magnetic Fe O4-silica-poly (. Gamma. -benzyl-l-glutarate) composite microspheres [ J)]Reactive and Functional Polymers, 2011, 71 (10): 1040-1044.). This method is to link the extractant and the inert matrix by chemical bonds, but the presence of aminosilanes introduces carbon chains, which leads to a decrease in irradiation stability. The impregnation method is to leave TODGA at SiO by physical action using intermolecular forces 2 A surface. In most literature concerning impregnation methods, experiments were carried out on SiO 2 Coating a layer of polymerized film of styrene and divinylbenzene on the surface to increase active sites, thus obtaining SiO 2 P particles (see (1) Hoshi H, wei Y Z, kumagai M, et al Group separation of trivalent minor actinides and lanthanides by TODGA extraction chromatography for radioactive waste management [ J)]. Journal of alloys and compounds, 2004, 374(1-2): 451-455. ②Wei Y, Kumagai M, Takashima Y, et al. Studies on the separation of minor actinides from high-level wastes by extraction chromatography using novel silica-based extraction resins[J]Nuclear technology, 2000, 132 (3): 413-423). Research results show that the preparation of the styrene and divinylbenzene polymeric membrane has the problems of complex process, easy adhesion among particles and the like, and the stability of products prepared in different batches cannot be ensured.
Disclosure of Invention
The invention provides a new application of TODGA silicon-based resin, and simultaneously provides a method for preparing TODGA silicon-based resin, which can overcome the defects of the prior art.
The new application of the TODGA silicon-based resin is that the TODGA silicon-based resin is used for selectively adsorbing Am (III).
More preferably, one of the materials of the present invention for selective adsorption of Am (III) is to adsorb TODGA to SiO 2 On the particles.
The preparation method of the material for selectively adsorbing Am (III) comprises the following steps: firstly methanol is used for preparing spherical SiO with large specific surface area 2 Activating the particles, and then adding SiO 2 Vacuum drying to thoroughly remove methanol in the pore canal, and mixing SiO 2 Microsphere, siO 2 Ethanol and SiO with the mass of 30-50 times of that of the microsphere 2 Uniformly mixing 10-50% of TODGA by mass, and sufficiently oscillating for more than 12 hours at room temperature to enable the TODGA to be on SiO 2 And (3) after the surface reaches adsorption equilibrium, maintaining a water bath at 60-75 ℃ after oscillation is finished, keeping ethanol at a relatively uniform and slow rate, evaporating the ethanol, washing the evaporated material with ultrapure water, and drying at 50-80 ℃ to obtain the TODGA solid-phase silicon-based resin.
The simulation test related to the invention shows that the TODGA has strong adsorption effect on Am-241 and other nuclides, and has excellent high acid resistance, and TODGA and SiO are used for preparing the catalyst 2 The solid-phase resin prepared by combining is a very potential material which can be applied to the separation and enrichment of Am-241 in radioactive waste liquid.
The invention adopts mesoporous SiO with large specific surface area 2 The microsphere is directly impregnated, which avoids the defects and defects generated in the preparation in the prior art, not only retains SiO 2 As a common substance, the material has the characteristics of low price, easy acquisition and stable physical and chemical properties, and simultaneously has the advantages of good irradiation stability and high mechanical strength.
Drawings
FIG. 1 is an infrared spectrum of the material of the present invention.
Fig. 2 is a scanning electron microscope image of the material of the present invention.
FIG. 3 is a thermogravimetric curve of a material according to the present invention.
FIG. 4 is a graph showing the effect of acidity on Eu (III) adsorption performed by the material of the present invention.
FIG. 5 is a graph showing the initial concentration effect of Eu (III) adsorption by the material of the present invention.
FIG. 6 is a graph showing the effect of contact time on Eu (III) adsorption by the material of the present invention.
FIG. 7 is a graph showing the effect of ionic strength on Eu (III) adsorption by the material of the present invention.
FIG. 8 is a graph showing the effect of different ion selectivities on Eu (III) adsorption by the materials of the present invention.
Detailed Description
Eu and Am, elements 63 and 95 belong to the lanthanide series and actinide series. Eu outer layer electrons are distributed as [ Xe ]4f76s2, am outer layer electrons are distributed as [ Rn ]5f77s2, an isotope tracer method is commonly used for analysis of isotopes 241Am at present, and a commonly used tracer is 243Am which is a manually synthesized nuclide, is not easy to obtain, has strong radioactivity and high toxicity, and is not beneficial to long-time operation of analysts. Eu (III) is a trivalent lanthanide, is in the same group as Am (III), has similar ionic radii and has certain similarity in chemical behavior. The invention subject group systematically compares coprecipitation behaviors of Am and Eu under different coprecipitation agents and adsorption and elution behaviors on TRU resin and DGA resin, and explains consistency of coprecipitation behaviors by referring to related thermodynamic parameters (Visual MINTEQ) of Am and Eu, and explains consistency of Am and Eu column behaviors by combining theoretical calculation and adsorption mechanism. Therefore, eu is adopted as an analogue of Am in the experimental process to explore the adsorption behavior of the Eu on the TODGA silicon-based resin, so that a reference is provided for separation of the resin applied to Am-241.
The present invention is explained below in connection with a simulation experiment in which Eu is used as a non-isotopic tracer for Am.
1. Preparation of TODGA solid-phase silicon-based resin
In a 50 mL polytetrafluoroethylene bottle, 1.0 g large specific surface area silica microspheres are weighed, 40 mL absolute ethyl alcohol is added, 0.5 g TODGA is weighed and mixed uniformly, and 200 r/min oscillation 12h is carried out at room temperature. After the shaking was completed, the ethanol solution was evaporated to dryness in a water bath at 65 ℃. The TODGA silicon-based resin is prepared by four times of washing with 200 mL ultra-pure water, and the washed resin is dried in an oven at 60 ℃.
TODGA is also commercially available directly from the Barling technology Co.
2. Adsorption test results and characterization of the inventive materials
1) Preparing a solution: (1) 3M HNO 3 Solution preparation: preparation of 3M HNO with concentrated nitric acid and ultra pure water 3 A solution. Using a measuring cylinder to take 385 mL ultrapure water into a polytetrafluoroethylene bottle with a concentration of 500 mL, adding 105 mL concentrated nitric acid into the polytetrafluoroethylene bottle, and shaking the mixture uniformly for later use.
(2) Preparing 1000 ppm Eu (III) mother solution: 0.1467 g Eu (NO) 3 ) 3 ·6H 2 O reagent in a beaker, adding a certain amount of 3M HNO 3 Dissolving, transferring to 50 mL volumetric flask after dissolving, and adding 3M HNO 3 And (3) fixing the volume, shaking uniformly, and transferring the dissolved solution to a reagent bottle for standby.
(3) 1.2 NaNO of 1.2M 3 Preparing a solution: weighing 1.02 g NaNO 3 With a certain amount of 3M HNO 3 Dissolving, transferring into 10 mL volumetric flask after dissolving, and adding 3M HNO 3 And (3) fixing the volume, shaking uniformly, and transferring the dissolved solution to a reagent bottle for standby.
(4) Preparing a gradient concentration nitric acid solution: 9.73, 9.10, 8.40, 7.70, 7.00, 6.30, 5.60, 4.90 and 4.20 and mL ultrapure water are respectively taken by a pipetting gun, and 0.07, 0.70, 1.40, 2.10, 2.80, 3.50, 4.20, 4.90 and 5.60 and mL concentrated nitric acid are respectively taken by pipetting, thus obtaining 0.1, 1, 2, 3, 4, 5, 6, 7 and 8M HNO 3 The solution is shaken up for standby. 0.01 M HNO 3 With 0.1M HNO 3 Diluting.
2) The specific adsorption test flow is as follows:
adding 1000 ppm Eu (III) mother liquor and 3M HNO with preset volume into a 10 mL test tube 3 (or other concentration of nitric acid solution), naNO 3 The solution or series of interfering ion standard solutions are used for preparing the stock solution of each static adsorption test. Weighing 0.02 g of TODGA silicon-based resin in a 10 mL centrifuge tube, adding 5.00 g of the resinAnd (3) corresponding to the mL of stock solution. And (5) taking out the centrifuge tube after oscillating for a preset period of time at room temperature.
The stock solution was diluted with ultrapure water to a concentration range in which ICP-OES can measure. And (3) carrying out solid-liquid separation on the liquid in the centrifuge tube by using a nylon filter membrane with the pore diameter of 0.22 mu m, and diluting a certain amount of supernatant by using ultrapure water to be the same multiple as the original liquid. The stock solution and the concentration after adsorption were measured by ICP-OES.
3) The relevant tests and results are as follows: (1) infrared spectrogram: unmodified SiO 2 TODGA silicon-based resin and 3M HNO 3 The infrared spectrum of the TODGA silicon-based resin after 5 days of acid soaking is shown in figure 1. SiO (SiO) 2 In the spectrum of 1095 cm -1 、811 cm -1 、472 cm -1 、960 cm -1 Si-O-Si stretching vibration peaks, si-O symmetrical vibration and bending vibration peaks and Si-O-H stretching vibration appear respectively; TODGA silicon-based resin for removing the above SiO 2 Out of the characteristic peak, 1650 cm -1 Amide bond at 1470 and 1470 cm -1 、2960 cm -1 、2924 cm -1 、2855 cm -1 C-H stretching vibration peak. The appearance of amide bonds and C-H vibrational peaks indicates that TODGA functionality is present at SiO 2 On the above, successful impregnation was demonstrated. The characteristic peak of TODGA is not changed after acid leaching, which proves that the sample can be obtained in 3M HNO 3 The following has a certain structural stability.
(2) Scanning electron microscope image: the scanning electron microscope characterization diagram of the silicon-based resin before and after acid leaching is shown in figure 2, at 3M HNO 3 SiO before and after pickling 2 The spherical structure of the material is not changed, and the combination of the infrared analysis results proves that the material can be used in a high-acid environment.
(3) Thermal gravimetric curve: unmodified SiO 2 The thermogravimetric curve of the TODGA silicon-based resin is shown in FIG. 3, siO 2 The thermogravimetric curve loses H at 100 DEG C 2 The quality does not change obviously after O; after the TODGA silicon-based resin is subjected to 210 ℃, the extractant TODGA starts to lose weight, and the content of the extractant TODGA accounts for about 40% of the resin, which shows that the material has certain thermal stability.
(4) The effect of system acidity on adsorption, see fig. 4: in the experiment of the invention, 0.5. 0.5 pp of the nitric acid with gradient concentration is preparedm Eu (III) solution is used as a stock solution. The results show that the material is prepared in 8M HNO 3 The lower adsorption rate can reach 99 percent.
(2) The effect of initial concentration on adsorption, see fig. 5: in the experiments of the invention, 3M HNO is used 3 And 1000 ppm Eu (III) solution 5, 10, 20, 50, 100, 200, 400 ppm Eu (III) solution as stock solution. Experimental data are simulated by using a Langmuir theoretical model, and the maximum adsorption capacity of the material is 64.0 mg/g.
(3) The effect of contact time on adsorption, see fig. 6: from the graph, the adsorption rate of the material is fast and the adsorption rate is rapidly increased within the first 10 min; adsorption reaches equilibrium after 60 min, which is a rapid equilibrium process.
(4) The effect of ionic strength on adsorption, see fig. 7: in the experiments of the invention, 3M HNO is used 3 1000 ppm Eu (III) solution and 1.2M NaNO 3 Preparation of 0.5 ppm Eu (III) and 0.2, 0.4, 0.6, 0.8, 1.0M NaNO 3 As a result of raw solution research, the increase of the ionic strength has little effect on the adsorption performance of the material.
(5) The effect of ion selectivity on adsorption, see figure: in the experiments of the invention, 3M HNO is used 3 A solution of 0.5 ppm Eu (III) and a solution of 1, 10, 100, 500 times the number of moles of Eu (III) in the form of a solution of 1000 ppm Eu (III) and a 1000 ppm interfering ion mother liquor were prepared as a stock solution. The influence of the interfering ions on the adsorption behavior of Eu (III) on the resin is investigated by forming mixed solutions of Cs (I), sr (II), ce (III) and Zr (IV) and target metal ions Eu (III) respectively. The research result shows that as the concentration of impurity metal ions increases, the separation behaviors of different interfering ions on Eu (III) are slightly different: cs (I) does not substantially affect Eu (III) adsorption; ce (iii), zr (iv) and Sr (ii) slightly reduce the adsorption of Eu (iii) by the material, but when Sr (ii) concentration is 500 times that of Eu (iii), the Eu (iii) adsorption rate can still reach 75%.
The data show that the material has excellent selectivity to Eu (III) in a metal ion mixed system.
Claims (2)
1. Be used for selectively adsorbing Am (III) materialThe preparation method of the material is characterized in that methanol is firstly used for preparing spherical SiO with large specific surface area 2 Activating the particles, and then adding SiO 2 Vacuum drying to thoroughly remove methanol in the pore canal, and mixing SiO 2 Microsphere, siO 2 Ethanol and SiO with the mass of 30-50 times 2 Uniformly mixing 10-50% of TODGA by mass, and oscillating at room temperature for 12-h to enable the TODGA to be on SiO 2 And (3) after the surface reaches adsorption equilibrium, maintaining a water bath at 60-75 ℃ after oscillation is finished, keeping ethanol at a relatively uniform and slow rate, evaporating the ethanol, washing the evaporated material with ultrapure water, and drying at 50-80 ℃ to obtain the TODGA silicon-based resin.
2. The selective adsorbent Am (III) material prepared by the method of claim 1.
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Citations (6)
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JP2003185792A (en) * | 2001-12-19 | 2003-07-03 | Japan Atom Energy Res Inst | Method of extracting and separating americium from lanthanoid |
JP2003215292A (en) * | 2002-01-22 | 2003-07-30 | Inst Of Research & Innovation | Method for separating and recovering americium, curium, and rare-earth element |
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JP2010271243A (en) * | 2009-05-22 | 2010-12-02 | Japan Atomic Energy Agency | N,n,n',n'-tetraalkyl-3,6-dioxaoctane-1,8-diamide and extractant for solvent-extracting actinide element and lanthanide element from high level radioactive waste liquid including n,n,n',n'-tetraalkyl-3,6-dioxaoctane-1,8-diamide |
US8354085B1 (en) * | 2012-03-16 | 2013-01-15 | U.S. Department Of Energy | Actinide and lanthanide separation process (ALSEP) |
JP2018123373A (en) * | 2017-01-31 | 2018-08-09 | 国立研究開発法人日本原子力研究開発機構 | Selective separation method of metal element and separation unit |
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US7157022B2 (en) * | 2002-09-30 | 2007-01-02 | .Pg Research Foundation, Inc. | Multivalent metal ion extraction using diglycolamide-coated particles |
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JP2003185792A (en) * | 2001-12-19 | 2003-07-03 | Japan Atom Energy Res Inst | Method of extracting and separating americium from lanthanoid |
JP2003215292A (en) * | 2002-01-22 | 2003-07-30 | Inst Of Research & Innovation | Method for separating and recovering americium, curium, and rare-earth element |
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JP2010271243A (en) * | 2009-05-22 | 2010-12-02 | Japan Atomic Energy Agency | N,n,n',n'-tetraalkyl-3,6-dioxaoctane-1,8-diamide and extractant for solvent-extracting actinide element and lanthanide element from high level radioactive waste liquid including n,n,n',n'-tetraalkyl-3,6-dioxaoctane-1,8-diamide |
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