CN114130367A - Magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil - Google Patents
Magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil Download PDFInfo
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- CN114130367A CN114130367A CN202111429122.9A CN202111429122A CN114130367A CN 114130367 A CN114130367 A CN 114130367A CN 202111429122 A CN202111429122 A CN 202111429122A CN 114130367 A CN114130367 A CN 114130367A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- G21F9/28—Treating solids
- G21F9/30—Processing
Abstract
The invention discloses a cleaning magnetic adsorption material for treating radioactive contaminated soil and a preparation method thereof. Using deionized water to mix FeCl3·6H2O、FeCl2·4H2O、NH3·H2Preparing a mixed solution D from O; the mixture D was magnetically separated with a magnet and dried by washing to obtain substance J. Preparing 37% hydrochloric acid into a solution K1 by using deionized water; adding chitosan into K1 to prepare a mixed solution L; dropwise adding a mixed solution M prepared from potassium tripolyphosphate into the mixed solution L to prepare a mixed solution N, and centrifuging and freeze-drying to obtain a substance O. Preparing sodium alginate into a mixed solution P by using deionized water; preparing a mixed solution P3 from a substance J, methyl orthosilicate, a substance O and the mixed solution P; the mixed solution P3 is dripped into CaCl with the mass concentration of 2 percent2In the solution, the solution is added with a solvent,filtering through a filter screen with the aperture of 5mm to obtain a substance Q; and (3) cleaning the substance Q with deionized water, and drying to obtain the substance, namely the magnetic adsorption material for cleaning and decontaminating soil.
Description
Technical Field
The invention belongs to the technical field of radionuclide pollution restoration and treatment, and particularly relates to a magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil.
Background
The aim of repairing the radioactive contaminated soil is to reduce the concentration of radioactive nuclide in the soil to the maximum extent or fix and stabilize the radioactive nuclide so as to block the migration and transformation of the radioactive nuclide in the soil. In order to guarantee the using function of soil after restoration, the research based on the restoration purpose of the soil is an environmental improvement problem which needs to be broken urgently in the world nowadays. In the repairing technology of the radioactive contaminated soil, an adsorption method has the characteristics of simple and easy operation, controllable preparation cost, good nuclide removing effect and the like, so that the adsorption method is a quite wide repairing method in the contaminated soil treatment process.
The magnetic adsorption material is a magnetic material having an adsorption effect on a specific pollutant, or an adsorption material which is modified by using different types of functional groups to have an adsorption effect on a specific pollutant or enhance the physical and chemical stability of the adsorption material. At present, common magnetic materials comprise nanometer zero-valent iron, ferroferric oxide, hematite magnetite, magnetic graphene materials, magnetic core-shell composite materials and the like; the adsorbent material may be classified into inorganic adsorbent, organic adsorbent, composite adsorbent and biological adsorbent according to the type of the main material, and specifically includes natural minerals, natural polysaccharides, carbon materials, metal compounds, metal organic frames, and the like. The natural clay mineral material has the characteristics of low price, easy obtaining, large specific surface area, strong ion exchange capacity, small environmental pollution and the like, is deeply concerned by numerous scholars at home and abroad in the research of the recovery and utilization of nuclides, and relates to objects mainly comprising zeolite, talc, sepiolite, montmorillonite and diatomite; the substances have rich yield resources, but the treatment effect is generally low. Carbon materials mainly relate to activated carbon, carbon nanotubes, graphene, biochar and the like, have few selectivity on pollutant adsorption effects, and are limited by high treatment cost in practical application. The metal compounds and metal organic frameworks generally have ultrahigh specific surface area and porosity, can provide active metal sites for target pollutants, but lose advantages in large-scale practical disposal due to complicated preparation procedures and high application cost.
The natural polysaccharide substance mainly comprises cellulose, chitin and chitin derivative chitosan, wherein the chitosan has excellent complexation effect on metal ions because molecular chains contain a large amount of active amino and hydroxyl, and in addition, the novel chitosan derivative with different characteristics can be generated through various modes such as carboxylation reaction, esterification reaction, acylation reaction, etherification reaction, grafting reaction, crosslinking reaction and the like; the natural polymer has the advantages of higher plasticity, lower application cost, better biocompatibility and stronger biodegradability, and becomes a research hotspot for repairing the radioactive contaminated soil. However, the existing form of a single magnetic nanoparticle is unstable, oxidation reaction is very easy to occur under the naked condition, so that the magnetism and the dispersibility of the magnetic nanoparticle are greatly reduced, while pure chitosan has the characteristics of low solubility and insignificant selectivity, and in consideration of the properties of convenient application, recoverability and the like of the repair material, the research on the novel magnetic adsorption material for cleaning and decontaminating the radioactive contaminated soil still needs to be further enhanced, and the research on the preparation process of the magnetic adsorption material for cleaning and decontaminating the radioactive contaminated soil is still lacked.
Disclosure of Invention
The invention aims to provide a magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil. The method comprises the following specific steps:
(1) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution A;
(2) 0.0639mol of FeCl was added to the solution A2·4H2O, stirring for 30min under the condition of 800r/min to obtain a solution A1;
(3) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution B;
(4) 0.1120mol of FeCl was added to the solution B3·6H2O, stirring the mixture at the speed of 800r/min for 30min to obtain solution B1;
(5) adding the solution B1 into the solution A1, placing the solution in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, and violently stirring for 30min at the speed of 600r/min to obtain a mixed solution C;
(6) rapidly adding 120mL of ammonia water into the mixed solution C, placing the mixed solution C in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, continuously introducing nitrogen at the gas flow rate of 130L/h, and stirring the mixed solution C for 3h at the rotating speed of 600r/min to obtain a mixed solution D;
(7) cooling the mixed solution D to room temperature, performing magnetic separation on a black product in the three-neck flask by adopting strong magnet, and removing supernatant to obtain a mixture E;
(8) adding 300mL of deionized water into the mixture E, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture F;
(9) adding 300mL of deionized water into the mixture F, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture G;
(10) adding 300mL of absolute ethyl alcohol into the mixture G, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture H;
(11) adding 300mL of absolute ethyl alcohol into the mixture H, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture I;
(12) drying the mixture I at 60 ℃ for 12h to obtain a substance J;
(13) adding 300mL of deionized water into a beaker with the volume of 500mL, and dropwise adding 3mL of hydrochloric acid with the mass percentage concentration of 37% into the beaker under the condition of slow stirring to obtain a solution K;
(14) injecting the solution K into a 1000mL volumetric flask in a drainage mode, and fixing the volume to a scale mark by using deionized water to obtain a solution K1;
(15) adding 25g of chitosan into the solution K1, and stirring for 4 hours at the speed of 800r/min to obtain a mixed solution L;
(16) adding 150mL of deionized water into a beaker with the volume of 500mL, then adding 75g of potassium tripolyphosphate into the beaker, and stirring the mixture for 15min under the condition of 800r/min to obtain a mixed solution M;
(17) dropwise adding the mixed solution M into the mixed solution L, and stirring for 12 hours at the speed of 800r/min to obtain a mixed solution N;
(18) centrifuging the mixed solution N for 5min at 7000 rpm, discarding the supernatant, and drying the lower layer of residual solid in a freeze dryer for 24h to obtain a substance O;
(19) adding 300mL of deionized water into a conical flask with the volume of 500mL, placing the conical flask in a constant-temperature magnetic stirring water bath kettle at the temperature of 75 ℃, adding 3g of sodium alginate after the temperature of the deionized water in the conical flask rises to 75 ℃, and stirring for 15min at the speed of 800r/min to obtain a mixed solution P;
(20) adding 5g of the substance J into the mixed solution P, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P1;
(21) adding 0.8g of methyl orthosilicate into the mixed solution P1, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P2;
(22) adding 10g of substance O into the mixed solution P2, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P3;
(23) the mixed solution P3 is dripped into 1000mL of CaCl with the mass percentage concentration of 2%2Standing the solution for 24h, and filtering the solution through a filter screen with the aperture of 5mm to obtain a substance Q;
(24) and (3) cleaning the substance Q with deionized water, and then placing the substance Q in a freeze dryer for drying for 24 hours to obtain the substance, namely the magnetic adsorption material for cleaning and decontaminating the radioactive contaminated soil.
The method has the advantages that the technical process for preparing the soil cleaning magnetic adsorption material is simple, and the prepared magnetic adsorption material is low in cost and good in treatment effect when used for treating the radioactive contaminated soil.
Detailed Description
The invention provides a magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil, and the implementation process is illustrated by an example.
Examples
The soil cleaning magnetic adsorption material is prepared by the following steps:
(1) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution A;
(2) 0.0639mol of FeCl was added to the solution A2·4H2O, stirring for 30min under the condition of 800r/min to obtain a solution A1;
(3) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution B;
(4) 0.1120mol of FeCl was added to the solution B3·6H2O, stirring for 30min under the condition of 800r/min to obtain a solution B1;
(5) adding the solution B1 into the solution A1, placing the solution in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, and violently stirring for 30min at the speed of 600r/min to obtain a mixed solution C;
(6) rapidly adding 120mL of ammonia water into the mixed solution C, placing the mixed solution C in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, continuously introducing nitrogen at the gas flow rate of 130L/h, and stirring the mixed solution C for 3h at the rotating speed of 600r/min to obtain a mixed solution D;
(7) cooling the mixed solution D to room temperature, performing magnetic separation on a black product in the three-neck flask by adopting strong magnet, and removing supernatant to obtain a mixture E;
(8) adding 300mL of deionized water into the mixture E, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture F;
(9) adding 300mL of deionized water into the mixture F, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture G;
(10) adding 300mL of absolute ethyl alcohol into the mixture G, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture H;
(11) adding 300mL of absolute ethyl alcohol into the mixture H, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture I;
(12) drying the mixture I at 60 ℃ for 12h to obtain a substance J;
(13) adding 300mL of deionized water into a beaker with the volume of 500mL, and dropwise adding 3mL of hydrochloric acid with the mass percentage concentration of 37% into the beaker under the condition of slow stirring to obtain a solution K;
(14) injecting the solution K into a 1000mL volumetric flask in a drainage mode, and fixing the volume to a scale mark by using deionized water to obtain a solution K1;
(15) adding 25g of chitosan into the solution K1, and stirring for 4 hours at the speed of 800r/min to obtain a mixed solution L;
(16) adding 150mL of deionized water into a beaker with the volume of 500mL, then adding 75g of potassium tripolyphosphate into the beaker, and stirring the mixture for 15min under the condition of 800r/min to obtain a mixed solution M;
(17) dropwise adding the mixed solution M into the mixed solution L, and stirring for 12 hours at the speed of 800r/min to obtain a mixed solution N;
(18) centrifuging the mixed solution N for 5min at 7000 rpm, discarding the supernatant, and drying the lower layer of residual solid in a freeze dryer for 24h to obtain a substance O;
(19) adding 300mL of deionized water into a conical flask with the volume of 500mL, placing the conical flask in a constant-temperature magnetic stirring water bath kettle at the temperature of 75 ℃, adding 3g of sodium alginate after the temperature of the deionized water in the conical flask rises to 75 ℃, and stirring for 15min at the speed of 800r/min to obtain a mixed solution P;
(20) adding 5g of the substance J into the mixed solution P, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P1;
(21) adding 0.8g of methyl orthosilicate into the mixed solution P1, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P2;
(22) adding 10g of substance O into the mixed solution P2, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P3;
(23) the mixed solution P3 is dripped into 1000mL of CaCl with the mass percentage concentration of 2%2Standing in the solution for 24h, and passing through the pore sizeFiltering with a 5mm filter screen to obtain a substance Q;
(24) and (3) cleaning the substance Q with deionized water, and then placing the substance Q in a freeze dryer for drying for 24 hours to obtain the substance, namely the magnetic adsorption material for cleaning and decontaminating the radioactive contaminated soil.
The soil cleaning magnetic adsorption material obtained by the invention is added into a soil chemical cleaning reactor system to carry out treatment tests on the radioactive contaminated soil, and the results show that the system can effectively remove uranium in the contaminated soil, and when the initial content of uranium in the contaminated soil is 500mg/kg, the uranium in the treated soil can be reduced to 49 mg/kg.
Claims (1)
1. A magnetic adsorption material for cleaning and decontaminating radioactive contaminated soil is characterized in that the method for preparing the magnetic adsorption material is as follows:
(1) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution A;
(2) 0.0639mol of FeCl was added to the solution A2·4H2O, stirring for 30min under the condition of 800r/min to obtain a solution A1;
(3) adding 300mL of deionized water into a three-neck flask with the volume of 1000mL, placing the three-neck flask into a constant-temperature water bath kettle at the temperature of 75 ℃, and continuously introducing nitrogen into the three-neck flask at the gas flow rate of 130L/h for 30min to obtain a solution B;
(4) 0.1120mol of FeCl was added to the solution B3·6H2O, stirring for 30min under the condition of 800r/min to obtain a solution B1;
(5) adding the solution B1 into the solution A1, placing the solution in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, and violently stirring for 30min at the speed of 600r/min to obtain a mixed solution C;
(6) rapidly adding 120mL of ammonia water into the mixed solution C, placing the mixed solution C in a constant-temperature magnetic stirring water bath kettle at the temperature of 80 ℃, continuously introducing nitrogen at the gas flow rate of 130L/h, and stirring the mixed solution C for 3h at the rotating speed of 600r/min to obtain a mixed solution D;
(7) cooling the mixed solution D to room temperature, performing magnetic separation on a black product in the three-neck flask by adopting strong magnet, and removing supernatant to obtain a mixture E;
(8) adding 300mL of deionized water into the mixture E, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture F;
(9) adding 300mL of deionized water into the mixture F, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and discarding the supernatant to obtain a mixture G;
(10) adding 300mL of absolute ethyl alcohol into the mixture G, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture H;
(11) adding 300mL of absolute ethyl alcohol into the mixture H, stirring for 15min under the condition of 800r/min, performing magnetic separation by adopting strong magnet, and removing supernatant to obtain a mixture I;
(12) drying the mixture I at 60 ℃ for 12h to obtain a substance J;
(13) adding 300mL of deionized water into a beaker with the volume of 500mL, and dropwise adding 3mL of hydrochloric acid with the mass percentage concentration of 37% into the beaker under the condition of slow stirring to obtain a solution K;
(14) injecting the solution K into a 1000mL volumetric flask in a drainage mode, and fixing the volume to a scale mark by using deionized water to obtain a solution K1;
(15) adding 25g of chitosan into the solution K1, and stirring for 4 hours at the speed of 800r/min to obtain a mixed solution L;
(16) adding 150mL of deionized water into a beaker with the volume of 500mL, then adding 75g of potassium tripolyphosphate into the beaker, and stirring the mixture for 15min under the condition of 800r/min to obtain a mixed solution M;
(17) dropwise adding the mixed solution M into the mixed solution L, and stirring for 12 hours at the speed of 800r/min to obtain a mixed solution N;
(18) centrifuging the mixed solution N for 5min at 7000 rpm, discarding the supernatant, and drying the lower layer of residual solid in a freeze dryer for 24h to obtain a substance O;
(19) adding 300mL of deionized water into a conical flask with the volume of 500mL, placing the conical flask in a constant-temperature magnetic stirring water bath kettle at the temperature of 75 ℃, adding 3g of sodium alginate after the temperature of the deionized water in the conical flask rises to 75 ℃, and stirring for 15min at the speed of 800r/min to obtain a mixed solution P;
(20) adding 5g of the substance J into the mixed solution P, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P1;
(21) adding 0.8g of methyl orthosilicate into the mixed solution P1, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P2;
(22) adding 10g of substance O into the mixed solution P2, and stirring for 4 hours at the speed of 800r/min to obtain mixed solution P3;
(23) the mixed solution P3 is dripped into 1000mL of CaCl with the mass percentage concentration of 2%2Standing the solution for 24h, and filtering the solution through a filter screen with the aperture of 5mm to obtain a substance Q;
(24) and (3) cleaning the substance Q with deionized water, and then placing the substance Q in a freeze dryer for drying for 24 hours to obtain the substance, namely the magnetic adsorption material for cleaning and decontaminating the radioactive contaminated soil.
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Application publication date: 20220304 |