CN114653739A - Method for removing uranium in gravel-containing original rock loose sandy soil - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/02—Extraction using liquids, e.g. washing, leaching, flotation
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Abstract
The invention discloses a method for removing uranium from gravel-containing original rock loose sandy soil, and belongs to the technical field of contaminated soil remediation. Adding a leaching solution and an oxidant into gravel-containing raw rock loose sandy soil, oscillating at normal temperature, separating sandy soil from supernatant through centrifugation, washing the separated sandy soil twice, combining the supernatant, filtering, and detecting filtrate; wherein the oxidant is potassium permanganate or hydrogen peroxide, and the mass ratio of the oxidant to the gravel-containing original rock loose sandy soil is (0.005-0.02): 3. Compared with biological decontamination and physical decontamination methods, the method has the advantages of simple operation, low treatment cost, wide applicable uranium concentration range, high uranium extraction rate and the like.
Description
Technical Field
The invention belongs to the technical field of contaminated soil remediation, and particularly relates to a method for removing uranium in gravel-containing original rock loose sandy soil.
Background
With the development of nuclear industry, radioactive ores such as uranium are continuously mined, and although tailings residues are treated by a special process, uranium in the tailings can be released again, and the uranium enters soil and finally enters deeper soil layers or underground water to pollute the soil or the underground water. The soil is the first barrier to prevent uranium from entering groundwater and is therefore of great significance in uranium contaminated soil remediation.
At present, the uranium contaminated soil remediation methods comprise physical remediation, biological remediation and chemical remediation. The physical remediation method refers to a method for achieving remediation purposes by changing the physical properties of soil, and is generally used for treating low-concentration and small-range uranium soil. The bioremediation method is a method for extracting uranium in soil by absorbing, enriching, extracting or filtering the uranium in the soil by using a microorganism or plant system, and has the defects of long period, high cost, uncontrollable removal rate and the like. The chemical remediation method mainly aims at adding a chemical reagent into soil, and utilizes the adsorption, oxidation reduction and complexing chelation of the chemical reagent to convert uranium in the soil into hexavalent uranium to be precipitated so as to achieve the purpose of decontamination. The method can extract high-concentration uranium from soil, and has the advantages of high efficiency, process operability and the like. Uranium, however, binds tightly to soil and is difficult to remove, and its mobility and bioavailability, like other contaminants, depends to a large extent on the type of complexation it forms in the soil and the nature of the soil components that bind. Aiming at the loose sandy soil which is alkaline and contains sandstone and protorock in a certain area and has high uranium content, a uranium removal method is formulated. No specific uranium removal method has been reported for this characteristic of soil.
Disclosure of Invention
The invention aims to provide a method for removing uranium from gravel-containing crude rock loose sandy soil, which has the advantages of simple operation, low treatment cost, wide applicable uranium concentration range, high uranium extraction rate and the like compared with a biological decontamination and physical decontamination method.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for removing uranium from gravel-containing raw rock loose sandy soil comprises the steps of adding leachate and an oxidant into gravel-containing raw rock loose sandy soil, oscillating at normal temperature, separating sandy soil from supernatant through centrifugation, washing the separated sandy soil twice, combining the supernatant, filtering, and detecting filtrate; wherein the oxidant is potassium permanganate or hydrogen peroxide, and the mass ratio of the oxidant to the gravel-containing original rock loose sandy soil is (0.005-0.02): 3. Preferably 0.02: 3.
Further, the loose sandy soil containing the gravel original rock needs to be pretreated before use, and specifically comprises the following steps: drying the gravel-containing original rock loose sandy soil at 40 ℃, sieving the gravel-containing original rock loose sandy soil with a sieve with the particle size of 2cm, then drying the gravel-containing original rock loose sandy soil for 2 to 4 hours at the temperature of 105 ℃ and 110 ℃, uniformly mixing, and continuously sieving to obtain the gravel-containing original rock loose sandy soil with the particle size of 200 meshes.
Furthermore, the uranium content in the gravel-containing crude rock loose sandy soil is 100.79-5083.54 Bq/kg.
Further, the concentration of the leaching solution is 0.2-0.6mol/L, preferably 0.2mol/L, and the solid-to-liquid ratio of the leaching solution to the gravel-containing original rock loose sandy soil is (5-20): 1, preferably 20: 1.
Further, the leachate is sodium bicarbonate or sodium citrate.
Further, the oscillation speed is 160rpm, and the time is 408 h.
The binding morphology of uranium in soil directly affects the choice of soil decontamination methods. The bonding form of uranium in soil includes: ion exchange state, carbonate exchange state, iron manganese oxide combination state, organic combination state and residue state. The uranium in the soil can be efficiently removed by general physical methods of ion exchange state such as water washing. Carbonate bound, ferrimanganite bound and organically bound require strong chemical treatment. Therefore, the invention takes the pretreated gravel-containing original rock loose sandy soil as a raw material, and extracts uranium in an ion exchange state, a carbonate exchange state, a ferro-manganese oxide combination state, an organic combination state and a residue state in sequence according to the combination state of the uranium in the gravel-containing original rock loose sandy soil so as to judge the proportion of uranium in the soil in different combination states. The method comprises the following specific steps:
1. pretreatment of raw materials: taking gravel-containing crude rock loose sand 5cm from the earth surface as a sample (the uranium content is in the range of 100.79-5083.54 Bq/kg), drying, crushing, sieving with a sieve with the particle size of 2cm, drying at the temperature of 105 ℃ and 110 ℃ for 2-4h, mixing uniformly, sieving, and ball-milling until the particle size of the gravel-containing crude rock loose sand is 200 meshes.
2. Extraction of uranium in different binding morphologies:
1) extraction of uranium in ion-exchanged state: taking pretreated gravel-containing original rock loose sandy soil as a raw material, and adding 1mol/L CH3And adjusting the pH value of a COONa solution (an extracting agent) to 8, oscillating at room temperature for 3h, centrifuging at 9800rpm for 10min, removing the supernatant, repeating the operation, combining the supernatants, and fixing the volume to complete the extraction of the ion-exchange uranium, wherein the obtained precipitate is used as a raw material for the next extraction. The mass volume ratio of the raw material to the extracting agent is 1.5 g: 30 mL.
2) Extraction of uranium in a carbonate-bound state: adding 1mol/L CH into the precipitate obtained by the last extraction as a raw material3COONa solution, selecting CH3Adjusting pH to 5 with COOH, shaking at 50 deg.C for 5h, centrifuging with a centrifuge at 9800rpm for 10min, removing supernatant, repeating the operation, combining supernatants, and fixing volume.
3) Extraction of uranium in ferrimanganic oxide bonded state: adding CH with volume fraction of 25% into the precipitate obtained by the last extraction as raw material3COOH solution, adjusting pH to 2, shaking at 60 deg.C for 8h (wherein, CH3The COOH solution contains 0.04mol/L NH2OH HCl solution); then centrifuging with a centrifuge at 9800rpm for 10min, removing the supernatant, repeating the operation, combining the supernatants, and fixing the volume.
4) Extraction of uranium in an organically bound state: adding HNO into the precipitate obtained by the last extraction as a raw material3And 30% by volume of H2O2Shaking at 85 deg.C for 2h, and adding CH3COONH4Shaking at 65 deg.C for 8h, centrifuging at 9800rpm for 10min, removing supernatant, and weighingAnd (5) repeating the operation, combining the supernatant and fixing the volume.
5) Extraction of uranium in the residuum state: adding HNO into the precipitate obtained by the last extraction as a raw material3HF and H2O2Performing pre-digestion at 60 ℃ for 30min, performing microwave digestion, cooling, and adding HNO3Then, the mixture is centrifuged by a centrifuge at 9800rpm for 10min, the supernatant is removed, the operation is repeated, and the supernatants are combined to be constant volume.
Analyzing the obtained uranium-containing solutions with different binding forms to respectively obtain the uranium content of each binding form.
Compared with the prior art, the invention has the beneficial effects that:
1. aiming at the soil containing gravel original rock loose sandy soil, the invention confirms that the organic combination state of uranium and soil in the soil of the area is mainly the organic combination state, and the uranium accounts for 93 percent.
2. By exploring the extraction rate by four factors, namely the concentration of the leaching solution, the solid-liquid ratio, the time and the dosage of the oxidant, the influence is found to be as follows: the dosage of the oxidant is more than the solid-liquid ratio, the time is more than the concentration of the leaching solution, and the dosage of the oxidant has the greatest influence on the leaching rate. The extraction of the carbonate has high selectivity on uranyl, has small destructiveness on carbonate and layered silicate minerals in soil, and cannot have large destructive effect and small soil loss rate like a strong acid extractant.
3. Under the environment temperature, the concentration of the leachate bicarbonate is 0.2mol/L, the solid-to-liquid ratio is 1:20, the oxidant is 3mL, the leaching time is 408h, the leaching rate reaches 72.38%, the uranium content is reduced from 1179Bq/kg to 325Bq/kg, and the soil loss rate is 1%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a graph of the binding profile of different soil samples;
figure 2 is a graph of the efficiency of extraction of uranium from contaminated sandy soil over time for different concentrations of sodium bicarbonate.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
The content of uranium in a soil sample used by the invention is in the range of 100.79-5083.54 Bq/kg. The soil samples used in the following examples had a uranium content of 1179 Bq/kg.
Example 1
1. Soil collection and preparation: and (3) taking loose sand samples of the gravel-containing original rock at the depth of 5cm on the ground surface of different areas in the field, drying and crushing the samples at the temperature of 40 ℃, sieving the samples by using a sieve with the particle size of 2cm, drying the samples at the temperature of 105 ℃ and 110 ℃ for 2 to 4 hours, uniformly mixing the samples, sieving the samples, and performing ball milling until the particle size of the loose sand of the gravel-containing original rock is 200 meshes (74 mu m).
2. Extraction of uranium with different binding morphologies (2 replicates were set and averaged):
1) extraction of uranium in ion-exchanged state: 1.5g of pretreated gravel-containing crude rock loose sandy soil is placed in a centrifuge tube, and 30mL of CH with the concentration of 1mol/L is added3Adjusting the pH of a COONa solution (extracting agent) to 8, oscillating at room temperature for 3h, centrifuging at 9800rpm for 10min by using a centrifuge, removing a supernatant, washing the centrifuge tube twice by using 15mL of deionized water (pH 7), pouring the washing liquid into the original 100mL centrifuge tube, screwing a cover, continuing centrifuging at 9800rpm for 10min, removing the supernatant, pouring the two supernatants into the same 100mL centrifuge tube, diluting to a scale by using distilled water, shaking uniformly, weighing and reserving for analysis. This supernatant is defined as the ion-exchanged state, phase one.
2) Extraction of uranium in a carbonate-bound state: using the precipitate obtained by the last extraction as a raw material, and adding 30mL of CH with the concentration of 1mol/L3COONa solution, selecting CH3Adjusting the pH value of COOH to 5, oscillating at 50 ℃ for 5h, centrifuging at 9800rpm for 10min by using a centrifuge, removing the supernatant, washing the centrifuge tube twice by using 15mL of deionized water (pH 7), pouring the washing liquid into the original 100mL centrifuge tube, screwing a cover, continuously centrifuging at 9800rpm for 10min, removing the supernatant, pouring the two supernatants into the same 100mL centrifuge tube, diluting to a scale by using distilled water, shaking uniformly, weighing and reserving for analysis. This supernatant was defined as the carbonate bound state, phase two.
3) Extraction of uranium in ferrimanganic oxide bonded state: by the precipitate obtained by the last extractionTaking the starch as a raw material, and adding 30mL of CH with the volume fraction of 25%3COOH solution, adjusting pH to 2, shaking at 60 deg.C for 8h (wherein, CH3The COOH solution contained 0.04mol/L NH2OH HCl solution); then centrifuging for 10min at 9800rpm with a centrifuge, removing the supernatant, pouring the two supernatants into the same 100mL centrifuge tube, diluting to the scale with distilled water, shaking up, weighing and reserving for analysis. The supernatant is defined as the combined state of the iron and manganese oxides, i.e. phase three.
4) Extraction of uranium in an organically bound state: the precipitate obtained by the last extraction is taken as a raw material, and 4.5mL of HNO is added3And 7.5mL of 30% volume fraction H2O2After 2h shaking at 85 ℃ 7.5mL CH was added3COONH4Shaking at 65 deg.C for 8h, centrifuging at 9800rpm for 10min with a centrifuge, removing the supernatant, pouring the two supernatants into the same 100mL centrifuge tube, diluting to the desired scale with distilled water, shaking, weighing, and analyzing. This supernatant was defined as the organically bound state, phase four.
5) Extraction of uranium in the residuum state: taking the precipitate obtained by the last extraction as a raw material, and adding 15mL of HNO with the concentration of 68.1%315mL of 50% HF and 2mL of H2O2Performing pre-digestion at 60 ℃ for 30min, performing electric heating plate digestion (repeatedly digesting at 220 ℃ for 3 times, each time digesting for 3.5h), cooling, and adding 10mL of 2% HNO3Then, the mixture was centrifuged at 9800rpm for 10min by a centrifuge, the supernatant was removed, the two supernatants were poured into the same 100mL centrifuge tube, diluted to the scale with distilled water, shaken well and weighed for analysis. This supernatant was defined as the residue, phase five.
The uranium measuring method comprises the following steps: respectively filtering 2mL of the five phase constant volume solutions with 0.45 μm filter membrane, and collecting the filtrate233Analyzing and determining a sample by using a U isotope dilution-inductively coupled plasma mass spectrometry (ICP-MS) method232Th、234U、235U、236U and238u, determination based on the thorium hydrogen coefficient232Th pair233The magnitude of U interference is calculated according to an isotope dilution formula234U、235U、236U and238and (4) the content of U. For each extraction step, a sample-free solution (reagent blank) was also obtained by this procedure and its U concentration was analyzed, each time below the quantitation limit of the ICP-MS instrument.
The detection results are as follows:
soil marking: ion exchange state 0.138Bq/kg, carbonate binding state 0.370Bq/kg, iron manganese oxide binding state 1.202Bq/kg, organic binding state 1.683Bq/kg, residue state 2.886 Bq/kg.
Sample preparation: the ion exchange state is 0.610Bq/kg, the carbonate combination state is 15.894Bq/kg, the iron-manganese oxide combination state is 12.477Bq/kg, the organic combination state is 756.167Bq/kg, and the residue state is 30.200 Bq/kg.
The same analysis was performed using the soil as a control group, and the analysis results are shown in fig. 1. It can be seen that the uranium binding form ratio of the gravel-containing original rock loose sand sample (DU1-1 original sample) is very different, the uranium binding form in the soil of the area is mainly in an organic binding form and accounts for 93%, and the method for removing uranium is proved to be incapable of adopting the existing method for removing uranium from standard sample soil.
Example 2
The leaching test of uranium was carried out using the sample pretreated in example 1 as a raw material. The normal temperature is 25 ℃.
Adding gravel-containing crude rock loose sandy soil, sodium bicarbonate and potassium permanganate into a 50mL flask with a sealed headspace for reaction, oscillating at 160rpm at normal temperature, separating sandy soil from a supernatant through centrifugation, washing the separated sandy soil twice, combining the supernatants, filtering by using a pinhole syringe provided with a 0.45-micrometer filter head, analyzing the filtrate through ICP-MS, drying and weighing the residual soil, dissolving completely, and determining the concentration of residual soil uranium.
The solid-to-liquid ratio is the dosage ratio of the leachate sodium bicarbonate to the soil sample (gravel-containing original rock loose sandy soil). The amount of the soil sample was 3 g.
Four-factor three-level orthogonal experiments are carried out by taking four factors of leaching agent concentration, solid-liquid ratio, time and oxidant dosage as variables, and the four factors are shown in table 1.
TABLE 1 orthogonal experimental results of depleted uranium contaminated sandy soil with sodium bicarbonate as leaching agent
Figure 2 is a graph of the efficiency of extraction of uranium from contaminated sandy soil over time for different concentrations of sodium bicarbonate.
It can be seen that the range values R of the extraction rate of four factors of the leaching solution concentration, the solid-to-liquid ratio, the time and the oxidant dosage are respectively 5.08, 6.99, 5.61 and 11.47, and the result sequence is as follows: the dosage of the oxidant is greater than the solid-liquid ratio, the time is greater than the concentration of the leaching solution, and the leaching rate is influenced most by the dosage of the oxidant, mainly because the U (IV) substance cannot be dissolved by the carbonate, but can be oxidized into U (VI) by the oxidant, so that the solubility of the uranium is improved. The optimal leaching conditions in the experiment are as follows: the concentration of the leaching solution is 0.2mol/L, the solid-to-liquid ratio is 1:20, the time is 408h, the oxidizing agent is 20mg, and the extraction efficiency reaches 72.38%.
Rate of soil loss
m0G is the mass of the polluted soil before leaching; m is1The mass of the residue after leaching, g.
The mass of the soil before leaching in the experiment is 3g, and the mass of the residue after leaching is 2.97g, and the soil loss rate in the experiment is 1% through calculation.
Example 3
The same as example 1, except that the leachate sodium bicarbonate was replaced by sodium citrate.
As a result, the extraction efficiency after 408h was found to reach 53.57%. .
Example 4
The difference from example 1 is that the extraction efficiency reached 57.4% after shaking for 168 h.
Comparative example 1
The same as example 1, except that the leachate of sodium bicarbonate was replaced by nitric acid with a concentration of 8mol/L, and the extraction efficiency reached 88.45% after 168 hours of reaction. Although the extraction rate of the nitric acid is high, the nitric acid has great destructiveness to the soil, damages the soil matrix and causes certain difficulty for the soil to be restored to the original position.
Comparative example 2
The difference from example 1 is that the extraction efficiency achieved by replacing the leach solution sodium bicarbonate with sulfuric acid at a concentration of 3mol/L is 99.49%. The sulfuric acid soil has high loss rate and great soil destructiveness, so that the soil matrix is destroyed, and the soil is difficult to restore to the original position.
Comparative example 3
The dried soil was sub-sampled using a cone and quarter method, taking a mass of 1g per leaching experiment. Initial soil activity was determined by autoradiography. With 0.5MNH4HCO30.1M citric acid and 0.1M H2Solutions of SO4 were prepared in triplicate 10mL leaching experiments, carried out in 50mL vials sealed at the head space. The sample was allowed to react for one week on a shaking table with stirring at ambient temperature. After the reaction, the supernatant was separated from the bulk soil by filtration, and then acidified to pH 2 with concentrated nitric acid and analyzed by ICP-AES.
The method measures soil from two sites of MOD Eskmeals in the UK, and the maximum extraction amount is NH after 168h test4HCO3The total U extraction in a single batch was 42-50%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A method for removing uranium from gravel-containing raw rock loose sandy soil is characterized in that leachate and oxidant are added into the gravel-containing raw rock loose sandy soil, oscillation is carried out at normal temperature, sandy soil and supernatant are separated through centrifugation, the separated sandy soil is washed twice and the supernatant is combined, filtration is carried out, and filtrate is detected; wherein the oxidant is potassium permanganate or hydrogen peroxide, and the mass ratio of the oxidant to the gravel-containing original rock loose sandy soil is (0.005-0.02): 3.
2. The method as claimed in claim 1, wherein the loose sandy soil containing the gravel crude rock needs to be pretreated before use, and the method comprises the following steps: drying the loose sandy soil containing the gravel original rock at 40 ℃, sieving, drying at 110 ℃ for 2-4h at 105 ℃, mixing uniformly, and continuously sieving.
3. The method as claimed in claim 1, wherein the loose sandy soil of the gravel-containing crude rock has a particle size of 200 mesh.
4. The method as claimed in claim 1, wherein the uranium content in the gravel-containing crude rock loose sandy soil is 1277.79-5083.54 Bq/kg.
5. The method according to claim 1, wherein the concentration of the leaching solution is 0.2-0.6mol/L, and the solid-to-liquid ratio of the leaching solution to the gravel-containing original rock loose sandy soil is (5-20): 1.
6. the method of claim 5, wherein the leachate is sodium bicarbonate or sodium citrate.
7. The method according to claim 1, wherein the oscillation speed is 160rpm for 408 hours.
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