CN113952932A - Mineral product for adsorption and fixation of radionuclide, preparation and application thereof - Google Patents
Mineral product for adsorption and fixation of radionuclide, preparation and application thereof Download PDFInfo
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- CN113952932A CN113952932A CN202110911387.6A CN202110911387A CN113952932A CN 113952932 A CN113952932 A CN 113952932A CN 202110911387 A CN202110911387 A CN 202110911387A CN 113952932 A CN113952932 A CN 113952932A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/12—Naturally occurring clays or bleaching earth
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- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
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- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/16—Processing by fixation in stable solid media
- G21F9/162—Processing by fixation in stable solid media in an inorganic matrix, e.g. clays, zeolites
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a mineral product for adsorption and fixation of radioactive nuclide, and preparation and application thereof. The invention has the advantages of good adsorption and fixation effects of products, simple preparation method flow, convenient application method, short sintering time, low energy consumption and the like.
Description
Technical Field
The invention relates to the technical field of application of modified halloysite to adsorption and in-situ nuclide fixation.
Background
Nuclear power has been widely used in nuclear power plants and military applications. However, the development of the nuclear industry inevitably produces large amounts of spent fuel and nuclear waste, which poses serious challenges to the human living environment. One class of particular concern in high level waste disposal is the medium-life fission products, particularly90Sr (half-life period 28.8a) and137cs (half-life 30.2a), radiation beta and gamma. The high radioactive nuclear waste disposal in China adopts an internationally recognized deep geological disposal technical route, radionuclides are fixed or contained in a curing base material (glass, mineral or ceramic, ceramic-glass and the like) by means of the curing base material, and then the radionuclides are deeply buried in an underground disposal warehouse and are completely isolated from a biosphere as far as possible. However, the current synthesis of the solidified body usually requires complex equipment and process conditions, and has high raw material cost, long sintering time and high energy consumption.
Disclosure of Invention
The invention aims to solve the problems of high cost, long sintering time, high energy consumption and the like of the conventional product or method for fixing nuclide raw materials, and provides an organosilane-modified halloysite used as a nuclide adsorption and fixing object, which is simple to prepare, low in utilization cost and low in energy consumption. The invention also provides a preparation method and an application method of the product.
The invention firstly discloses the following technical scheme:
a mineral product for adsorption and immobilization of radionuclides, which is modified halloysite with amino and/or mercapto functional groups grafted on the surface.
The halloysite in the scheme is a 1:1 type dioctahedral phyllosilicate mineral, is generally in a tubular shape and has a high specific surface area.
According to some preferred embodiments of the invention, the modification is effected by an amino and/or mercapto group-containing organosilane, such as an aminosilane and/or a mercaptosilane.
The aminosilane in the above embodiment is represented by the formula R-Si-NH2The mercaptosilane refers to an organosilane having the formula R-Si-SH.
According to some preferred embodiments of the present invention, the organosilane is selected from one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltrimethoxysilane and mercaptopropyltrimethoxysilane.
The present invention further provides a process for the preparation of the above mineral product, which comprises:
and adding the halloysite into the solution of the organosilane, carrying out heating reflux reaction at 80-120 ℃ for 6-24h, and then separating and drying the obtained solid to obtain the mineral product.
According to some preferred embodiments of the invention, the ratio of the halloysite to the organosilane is: modifying 2-10 g halloysite by 1-10 mL of organosilane at normal temperature.
According to some preferred embodiments of the present invention, the solvent of the solution of the organosilane is selected from one or more of ethanol, ethanol-water mixture, toluene, n-hexane, and the like.
According to some preferred embodiments of the invention, the preparation method comprises:
dissolving 1-10 mL of the organic silane in 50-200 mL of an organic solvent to obtain an organic silane solution, adding 2-10 g of halloysite, stirring at the rotation speed of 200-800rpm, heating, and performing reflux reaction for 6-24 hours; and then, centrifugally separating, washing the solid product by using an organic solvent, and finally drying the obtained solid in an oven at the temperature of 100-120 ℃ to obtain the mineral product.
The invention further provides a method of use of the above mineral product, comprising:
the mineral product is added to an aqueous solution of a radionuclide to adsorb the nuclide.
Preferably, the addition amount is: the ratio of the mass of the mineral product to the volume of the nuclide aqueous solution is 0.5-1 g/L, wherein the concentration of the nuclide aqueous solution is 100-5000 mg/L.
Preferably, the adsorption process comprises: and adding the mineral product into the nuclide aqueous solution, adsorbing for 5-120 min under the stirring of 400-500 rpm, then performing centrifugal separation, and drying the solid product.
More preferably, the adsorption time is 30-60 min.
According to some preferred embodiments of the invention, the method of applying comprises:
and calcining the mineral product adsorbed with the radioactive nuclide at 900-1200 ℃ to fix the adsorbed nuclide.
Preferably, the temperature rise rate of the calcination is 10-50 ℃/min.
Preferably, the calcining time is 1-3 h.
The principle of the invention comprises: the organosilane is used for carrying out covalent grafting with hydroxyl on the surface of the halloysite, functional groups such as amino, sulfydryl and the like are introduced to the surface of the halloysite to form an effective adsorption site, in the adsorption process, a nuclide and a functional group on the surface of the halloysite are subjected to a complex reaction and adsorbed on the surface of a modified halloysite inner cavity, in the fixing process, the halloysite nanotube is subjected to collapse blocking under the heating condition of 900-1200 ℃, the nuclide adsorbed on the halloysite inner cavity is fixed in the nanotube, and the adsorption and in-situ fixation of the nuclide in the halloysite inner cavity are realized.
The invention has the following beneficial effects:
according to the preparation method, organosilane is fully utilized to carry out covalent grafting modification on the halloysite, and functional groups are introduced to the inner cavity surface of the halloysite, so that the inner cavity surface of the halloysite becomes a main adsorption site of nuclide; compared with other common halloysite modification methods (such as acid/alkali etching treatment, heat treatment, surfactant modification treatment and the like), organosilane grafting modification can stably graft a specific functional group on the inner cavity surface of the halloysite, so that site-specific adsorption of nuclides on the inner cavity surface of the halloysite is realized.
According to the application method, the two ends of the halloysite nanotube can collapse and be capped at 900-1200 ℃, so that adsorbed nuclides are fixed in the halloysite nanotube in situ; compared with other nuclide adsorption mineral materials (such as zeolite, synthetic mesoporous silica, montmorillonite and the like), the adsorption capacity of the organosilane modified halloysite to nuclides is higher, the high-temperature collapse seal end of the halloysite nanotube has a better curing effect on the adsorbed nuclides, and the leaching resistance of the fixed nuclides is more excellent.
Drawings
FIG. 1 is a chart of the infrared spectra of the organosilane modified halloysite sample of example 1
FIG. 2 shows NMR spectra of organosilane-modified halloysite samples of example 1
FIG. 3 shows the nerchinskite as such and a fixed nuclide Sr in example 12+And (5) a transmission electron microscope contrast image of the organosilane modified halloysite sample.
FIG. 4 is a graph of the organosilane modified halloysite sample vs. a mimic nuclide Sr in example 22+Adsorption profile of (a).
Detailed Description
The present invention is described in detail below with reference to the following embodiments and the attached drawings, but it should be understood that the embodiments and the attached drawings are only used for the illustrative description of the present invention and do not limit the protection scope of the present invention in any way. All reasonable variations and combinations that fall within the spirit of the invention are intended to be within the scope of the invention.
Example 1
An organosilane-modified halloysite was prepared by the following procedure:
(1) dissolving 10mL of 3-aminopropyltriethoxysilane in 200mL of ethanol, adding 10g of halloysite, heating and refluxing for 24h while stirring at 400rpm, then centrifuging, washing with ethanol solvent for 3 times, oven drying at 105 ℃, grinding, and sieving with a 100 mesh sieve. An organosilane modified halloysite sample was obtained. The structural characterization is carried out to obtain the infrared spectrogram of the halloysite before and after organosilane modification shown in figure 1 and the nuclear magnetic resonance spectrogram of the organosilane-modified halloysite shown in figure 2, and the halloysite has typical expansion vibration peaks of inner surface hydroxyl and inner hydroxyl respectively shown in figure 1Is located at 3698cm-1And 3626cm-1. 2933cm newly appeared after halloysite is grafted and modified by silane-1is-CH2The asymmetric stretching vibration of (a) indicates that the organosilane is successfully grafted on the halloysite surface. It can be seen from FIG. 2 that the organosilane is hydrolysed to form T2And T3And the structure is grafted on the surface of the halloysite through a dehydration condensation reaction with the hydroxyl on the surface of the halloysite.
Radionuclide Sr by the obtained organosilane-modified halloysite2+The adsorption of (a) is as follows:
(2) adding the obtained organosilane modified halloysite into a simulated radionuclide Sr2+The solution is added with 0.5g/(g/L) of modified halloysite mass/nuclide concentration meter, and is rapidly stirred for 2 hours at 500rpm by a stirrer, centrifugally separated, and the solid product is dried at 100 ℃.
Post-adsorption fixation was performed by the following procedure:
(3) putting the solid product obtained in the step (2) into a magnetic boat, putting the magnetic boat into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, calcining for 2h, naturally cooling to normal temperature, and taking out to obtain the fixed simulated radionuclide Sr2+Modified halloysite of (1).
And (3) performing transmission electron microscope characterization on the halloysite original sample (a) and the organosilane modified halloysite (b) obtained in the step (3) after Sr adsorption and in-situ calcination and fixation, wherein as shown in the attached drawing 3, the halloysite is in a hollow tubular shape before calcination, and the two ports of the calcined halloysite nanotube show obvious collapse and are converted into a solid rod shape from the hollow tubular shape.
Example 2
An organosilane-modified halloysite was prepared by the following procedure:
(1) dissolving 5mL of mercaptopropyl trimethoxysilane in 100mL of ethanol, adding 10g of halloysite, heating and refluxing for reaction for 12 hours under the stirring of 400rpm, then centrifugally separating, washing for 3 times by using an ethanol solvent, drying in an oven at 105 ℃, grinding and sieving by using a 100-mesh sieve. An organosilane modified halloysite sample was obtained.
Radionuclide by modification of halloysite with the obtained organosilaneSr2+The adsorption of (a) is as follows:
(2) adding the organosilane modified halloysite obtained in the step (1) into radionuclide Sr2+To the solution, 0.5g/(g/L) (based on modified halloysite mass/nuclide concentration) was added. Rapidly stirring at 500rpm for 2 hr with a stirrer, centrifuging, and oven drying the solid product at 100 deg.C. The adsorption curve is shown in figure 4, and the organosilane adsorbent can adsorb Sr for 30 min2+The adsorption amount of the adsorbent is up to 321 mg/g.
Post-adsorption fixation was performed by the following procedure:
putting the solid product obtained in the step (2) into a magnetic boat, putting the magnetic boat into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, calcining for 2h, naturally cooling to normal temperature, and taking out to obtain the fixed simulated radionuclide Sr2+Modified halloysite of (1).
Example 3
An organosilane-modified halloysite was prepared by the following procedure:
(1) dissolving 5mL of mercaptopropyl trimethoxysilane in 100mL of ethanol, adding 10g of halloysite, heating and refluxing for reaction for 12 hours under the stirring of 400rpm, then centrifugally separating, washing for 3 times by using an ethanol solvent, drying in an oven at 105 ℃, grinding and sieving by using a 100-mesh sieve. An organosilane modified halloysite sample was obtained.
Radionuclide Sr by the obtained organosilane-modified halloysite2+The adsorption of (a) is as follows:
(2) adding the organosilane modified halloysite obtained in the step (1) into radionuclide Sr2+To the solution, 1g/(g/L) (based on the mass of the modified halloysite per nuclide concentration) was added. Rapidly stirring at 500rpm for 2 hr with a stirrer, centrifuging, and oven drying the solid product at 100 deg.C. Adsorbing for 30 min according to the adsorption curve, the organosilane adsorbent can adsorb Sr2+The adsorption quantity of the adsorbent is 585 mg/g.
Post-adsorption fixation was performed by the following procedure:
putting the solid product obtained in the step (2) into a magnetic boat, putting the magnetic boat into a muffle furnace, heating to 1100 ℃ at the speed of 10 ℃/min, calcining for 2h, naturally cooling to normal temperature, and taking the productObtaining the fixed analog radionuclide Sr2+Modified halloysite of (1).
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (10)
1. Mineral product for radionuclide adsorption and immobilization, characterized in that: it is a modified halloysite with amino and/or mercapto functional groups grafted on the surface.
2. The mineral product according to claim 1, characterized in that: the modification is effected by organosilanes containing amino and/or mercapto groups.
3. The mineral product according to claim 2, characterized in that: the organosilane is selected from one or more of 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltrimethoxysilane and mercaptopropyltrimethoxysilane.
4. A method of producing a mineral product according to any one of claims 1 to 3, characterized in that: the method comprises the following steps: adding halloysite into a solution of organosilane containing amino and/or mercapto, carrying out heating reflux reaction at 80-120 ℃ for 6-24h, and then separating and drying the obtained solid to obtain the mineral product.
5. The method of claim 4, wherein: the ratio of the halloysite to the organosilane is as follows: and at normal temperature, modifying 2-10 g of halloysite by 1-10 mL of organosilane.
6. The method of claim 4, wherein: the solvent of the organosilane solution is one or more selected from ethanol, ethanol-water mixed solution, toluene and n-hexane.
7. The method of claim 4, wherein: the preparation method comprises the following steps: dissolving 1-10 mL of the organic silane in 50-200 mL of an organic solvent to obtain an organic silane solution, adding 2-10 g of halloysite, stirring at the rotation speed of 200-800rpm, heating, and performing reflux reaction for 6-24 hours; and then, centrifugally separating, washing the solid product by using an organic solvent, and finally drying the obtained solid in an oven at the temperature of 100-120 ℃ to obtain the mineral product.
8. Use of the mineral product according to any one of claims 1 to 3 and/or the mineral product obtained by the preparation process according to any one of claims 4 to 7, characterized in that: the method comprises the following steps: and adding the mineral product into an aqueous solution of radionuclide to adsorb nuclides.
9. The method of application according to claim 8, characterized in that: the ratio of the mass of the mineral product to the volume of the nuclide aqueous solution is 0.5-1 g/L, wherein the concentration of the nuclide aqueous solution is 100-5000 mg/L.
10. The method of application according to claim 8, characterized in that: and calcining the mineral product adsorbed with the radioactive nuclide at 900-1200 ℃ to fix the adsorbed nuclide in situ.
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