CN115148389A - Photocatalytic uranium removal method without catalyst - Google Patents
Photocatalytic uranium removal method without catalyst Download PDFInfo
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- CN115148389A CN115148389A CN202210766660.5A CN202210766660A CN115148389A CN 115148389 A CN115148389 A CN 115148389A CN 202210766660 A CN202210766660 A CN 202210766660A CN 115148389 A CN115148389 A CN 115148389A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a photocatalytic uranium removal method without a catalyst, and belongs to the technical field of environmental pollution treatment. According to the invention, organic matters are added into the uranium-containing wastewater, and the photocatalytic reaction is carried out after mixing and stirring, or hydrogen peroxide is added into the uranium-containing wastewater, and the reaction is carried out after mixing and stirring, so that uranium is removed from the wastewater. The method realizes the solidification effect of the uranyl ions by utilizing the photochemical characteristics of the uranyl ions, and has excellent selectivity and wide application prospect in uranium-containing wastewater treatment.
Description
Technical Field
The invention belongs to the technical field of environmental pollution treatment, and particularly relates to a photocatalytic uranium removal method without a catalyst.
Background
As a main fuel of nuclear energy, uranium resources have strategic significance for constructing a clean energy industry system. In areas with relatively poor uranium resources, the discovery of exploitable uranium resources, even the exploitation of unconventional uranium resources, is a basic guarantee for long-term development of nuclear energy. In addition, a large amount of uranium-containing waste liquid is generated during the circulation of nuclear fuel, and the nuclear waste liquid is properly treatedCan be developed sustainably. Among various methods for removing uranium, the photocatalytic method can reduce U (VI) which is easily dissolved in water into insoluble U (IV), so that the reductive immobilization of uranium is realized, and the method is an effective way for eliminating radioactive uranium pollution. The photocatalytic method has the advantages of environmental friendliness, high energy efficiency, simple operation and the like compared with other various methods, and researchers synthesize the TiO-containing material based on the method 2 、C 3 N 4 Many types of photocatalysts such as MOFs and COFs.
However, the design of the catalyst increases the investment of manpower and material resources, and the catalyst needs to be carried out under the protection of inert atmosphere, so that the practical application and large-scale popularization of the catalyst are greatly limited while extra cost is caused. In addition, the use of catalysts has a certain interfering effect on the analysis of the products and the mechanistic recognition of the photocatalytic process. Therefore, the development of a photocatalysis technology under the condition of proper air is important to research the photocatalysis mechanism through a proper method.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for removing uranium from wastewater by solidifying uranyl ions by using the photochemical characteristics of the uranyl ions.
In order to realize the purpose, the invention provides the following technical scheme:
a method for removing uranium by photocatalysis without a catalyst comprises the following steps of adding organic matters into uranium-containing wastewater, mixing and stirring the organic matters and the wastewater, and then carrying out photocatalytic reaction.
A method for removing uranium by photocatalysis without a catalyst comprises the following steps of adding hydrogen peroxide into uranium-containing wastewater, mixing and stirring the hydrogen peroxide and the wastewater, and reacting the hydrogen peroxide and the wastewater.
Furthermore, the uranium-bearing wastewater is wastewater containing uranyl ions, the pH value of the wastewater containing the uranyl ions is 1-10, and the concentration of the uranyl ions is 0.05-1 mM.
Further, the organic matter is an alcohol organic matter; the volume ratio of the organic matter to the uranium-containing wastewater is (0.1-10): 50.
further, the alcohol organic substance includes methanol and ethanol.
Further, the photocatalytic reaction is carried out in the atmosphere of air and/or nitrogen, and the light source is a xenon lamp light source.
Furthermore, the spectral range of the xenon lamp light source is full spectrum, and the intensity is 0-50 mW/cm 2 。
Further, the reaction is carried out in an air atmosphere, and the volume ratio of the hydrogen peroxide to the uranium-containing wastewater is (1-10): (10 to 100).
Compared with the prior art, the invention has the following beneficial effects:
(1) The method realizes the solidification effect of the uranyl ions by utilizing the photochemical characteristics of the uranyl ions under the condition of no additional catalyst.
(2) The invention can realize the solidification effect of uranyl ions by taking hydrogen peroxide as a reactant without illumination.
(3) The method for removing uranium from wastewater provided by the invention has excellent selectivity and wide application prospect in uranium-containing wastewater treatment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required in the embodiments will be briefly described below, 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 that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a graph showing the variation trend of the concentration of uranyl ions in uranium-containing wastewater in continuous photocatalytic solidification of uranium-containing wastewater in examples 1-2 of the present invention;
FIG. 2 is an appearance diagram of a product obtained by photocatalytic solidification of uranium-containing wastewater according to example 1-2 of the present invention, wherein (1) is a product under an air atmosphere, and (2) is a product under a nitrogen atmosphere;
FIG. 3 is an SEM image, a TEM image and an XRD image of a product obtained by photocatalytic solidification of uranium-containing wastewater according to examples 1-2 of the present invention, wherein a is an SEM image of the product under an air atmosphere, b is a TEM image of the product under an air atmosphere, c is an XRD image of the product under an air atmosphere, d is an SEM image of the product under a nitrogen atmosphere, e is a TEM image of the product under a nitrogen atmosphere, and f is an XRD image of the product under a nitrogen atmosphere;
FIG. 4 is a graph showing the change trend of the concentration of uranyl ions in the uranium-bearing wastewater after the uranium-bearing wastewater is photocatalytically cured for 20min in example 2 of the present invention;
FIG. 5 is a graph showing the change trend of the concentration of uranyl ions after the light irradiation is stopped 20min after the uranium-containing wastewater is photocatalytically cured in example 1-2 of the present invention;
FIG. 6 shows example 1 of the present invention and dropwise addition of H under dark conditions 2 O 2 XRD contrast patterns of the two obtained products;
FIG. 7 shows embodiment 3 of the present invention and modification H 2 O 2 A comparison graph of the amount of solution added to the solidification performance of uranium;
FIG. 8 shows the concentration of uranyl ions in uranium-containing wastewater obtained by photocatalytic curing of uranium-containing wastewater under different illumination intensities in example 1 of the present invention;
FIG. 9 shows the concentration of uranyl ions in uranium-containing wastewater obtained by photocatalytic solidification of uranium-containing wastewater at different methanol addition amounts in example 1 of the present invention;
FIG. 10 is a H-NMR chart of methanol before and after the photocatalytic reaction in example 1 of the present invention;
FIG. 11 is a schematic diagram of a reaction process of generating radicals by photoexcitation of uranyl ions;
FIG. 12 is a reaction mechanism roadmap for photocatalytic uranyl ion curing without an added catalyst;
fig. 13 is a graph of the effect of selective uranium removal in a multi-metal ionic system.
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.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between 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 description and examples are intended to be illustrative 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 invention relates to a photocatalytic uranium removal method without a catalyst, which comprises the following steps of adding organic matters into uranium-containing wastewater, mixing and stirring the organic matters and the uranium-containing wastewater, and carrying out photocatalytic reaction.
The invention relates to a photocatalysis uranium removal method without a catalyst, which comprises the following steps of adding hydrogen peroxide into uranium-containing wastewater, mixing and stirring the hydrogen peroxide and the uranium-containing wastewater, and reacting the hydrogen peroxide and the uranium-containing wastewater.
Further, the uranium-containing wastewater is wastewater containing uranyl ions, the pH value of the wastewater containing the uranyl ions is 1-10, and the concentration of the uranyl ions is 0.05-1 mM.
Further, the organic matter is an alcohol organic matter; the volume ratio of the organic matter to the uranium-containing wastewater is (0.1-10): 50.
further, the alcohol organic substance includes methanol and ethanol.
Further, the photocatalytic reaction is carried out in the atmosphere of air and/or nitrogen, and the light source is a xenon lamp light source.
Furthermore, the spectral range of the xenon lamp light source is full spectrum, and the intensity is 0-50 mW/cm 2 。
Further, the reaction is carried out in an air atmosphere, and the volume ratio of the hydrogen peroxide to the uranium-containing wastewater is (1-10): (10 to 100).
Example 1
Photocatalytic uranium removal without catalyst under air condition
50mL of uranyl nitrate solution was placed in a 100mL beaker, 2mL of methanol was added to give a uranyl ion concentration in the solution of 0.4mM, pH =5, and the intensity was 20mW/cm under air conditions 2 The xenon lamp light source of (a) irradiates the mixed liquid.
Example 2
Method for removing uranium by photocatalysis under conditions of no catalyst and nitrogen
50mL of uranyl nitrate solution was placed in a 100mL beaker, 2mL of methanol was added to give a uranyl ion concentration in the solution of 0.4mM, pH =5, and the intensity was 20mW/cm under nitrogen 2 The xenon lamp light source of (a) irradiates the mixed liquid.
Verification example 1
The intensity of 20mW/cm was used in examples 1 and 2 2 In the process of irradiating the mixed liquid by the xenon lamp light source, sampling is carried out once every 20min, and the uranyl ion concentration is determined by adopting an azoarsine III color development method, wherein the specific operation steps are as follows: 4ml of tartaric acid with the concentration of 1mol/L, 2.9ml of nitric acid solution with the concentration of 0.1mol/L and 0.8ml of azoarsine III solution with the mass fraction of 0.1% (nitric acid solution with the solvent of 0.01 mol/L) are mixed evenly in a centrifuge tube or a volumetric flask to prepare the color developing agent. Taking about 0.5ml of reaction solution from the reaction system each time, filtering by using a nylon injector and a nylon filter head with the aperture of 0.22 mu m to obtain clear liquid, taking 0.3ml of clear liquid, adding the clear liquid into a color developing agent, uniformly mixing, pouring the color developing agent into a glass cuvette, and performing absorption photometry by using a spectrophotometry at 652 nm. Measuring the absorbance at time tIs marked as I, I 0 Is the initial absorbance intensity; as shown in fig. 1, it was found that the concentration of uranyl ions in the solution gradually decreased with the passage of time.
After the photocatalytic reaction is finished, solid products are generated under the conditions of air and nitrogen, the generated solid products are recovered through high-speed centrifugation and dried in a vacuum drying oven, and the products are shown in figure 2, wherein (1) is a product under the air atmosphere, and (2) is a product under the nitrogen atmosphere, so that the product generated under the air atmosphere is a light yellow solid, and the product generated under the nitrogen atmosphere is black particles.
The products under air atmosphere and nitrogen atmosphere were characterized by SEM, TEM and XRD, and the results are shown in fig. 3, in which (1) is an SEM image of the product under air atmosphere, (2) is a TEM image of the product under air atmosphere, (3) is an XRD image of the product under air atmosphere, (4) is an SEM image of the product under nitrogen atmosphere, (5) is a TEM image of the product under nitrogen atmosphere, and (6) is an XRD image of the product under nitrogen atmosphere. The material with short rod-shaped or sheet-shaped structure generated under the air condition is the uranium filamentite (UO) through analysis 2 )O 2 ·2H 2 O, and the nano-particle substance generated in the nitrogen atmosphere is uranium dioxide UO 2 . Therefore, under the condition of no external photocatalyst, enrichment and removal of uranyl ions in the solution can be realized by utilizing the photochemical property of the uranyl ions.
Verification example 2
In example 2, an intensity of 20mW/cm was used 2 In the process of irradiating the mixed liquid by the xenon lamp light source, the irradiation is finished after 20min, then the atmosphere is changed into the air atmosphere, the reaction is continued, and the change trend of the concentration of the uranyl ions is tested. As a result, as shown in fig. 4, it was found that the uranyl ion concentration decreased rapidly after the nitrogen gas was introduced, but the uranyl ion concentration did not decrease continuously but increased first after the atmosphere was changed to air, and then decreased as the light irradiation continued. The result shows that the uranium dioxide generated by the reaction in the nitrogen atmosphere is unstable in the initial generation stage, and if air is introduced, the uranium dioxide can be oxidized into uranyl ions again and enter the solution, and the concentration of the uranyl ions can be reduced again by continuous illumination, so that the product generated in the air atmosphere is generatedAnd (4) forming a aquarius ore, so that solidification of the uranyl ions is realized.
Verification example 3
The intensity of 20mW/cm was used in examples 1 and 2 2 In the process of irradiating the mixed liquid by the xenon lamp light source, the irradiation is finished after 20min, the atmosphere of air or nitrogen is kept, and the concentration change of the uranyl ions is continuously monitored, and the result is shown in fig. 5.
Under the nitrogen atmosphere, the concentration of the uranyl ions in the illumination process is sharply reduced, and after the illumination is finished, the concentration of the uranyl ions is kept unchanged. The results show that the photoreaction mainly plays a role in reducing the concentration of uranyl ions in a nitrogen atmosphere, and generates short-lived substances such as free radicals and the like in the process of illumination, and induces conversion of the uranyl ions.
After the light irradiation is stopped under the air atmosphere, the concentration of uranyl ions continuously decreases for the next 100 minutes. The results show that there is a chemical reaction occurring in the absence of light, and thus a long-lived, highly stable material is produced during the light process.
Further confirmation of such a long-lived, highly stable substance is as follows: h is dripped into uranyl nitrate solution 2 O 2 Generating a light yellow solid, and recovering uranyl ions and H after the reaction is finished 2 O 2 The product is analyzed by XRD, and as a result, as shown in figure 6, the yellowish product and the uranyl ion solution photocatalysis product have the same crystal structure, and the substance with long service life and high stability is proved to be H 2 O 2 。
Example 3
Uranium removal under hydrogen peroxide and air conditions
50mL of uranyl nitrate solution was placed in a 100mL beaker so that the concentration of uranyl ions in the solution was 0.4mM and pH =5, and 10. Mu.LH was added dropwise thereto under air conditions 2 O 2 (35% by mass of an aqueous solution).
Change H 2 O 2 As a result of the addition of the solution, as shown in FIG. 7, it was found that H was added 2 O 2 Thereafter, the concentration of uranyl ions gradually decreasesAnd following H 2 O 2 The increase in the amount of addition and the increase in the rate of decrease indicate that H 2 O 2 The amount of (b) is a main factor affecting the reaction. This result indicates that H is generated by photochemical reaction 2 O 2 Velocity ratio H of 2 O 2 Fast reaction rate with uranyl ions, H 2 O 2 The chemical reaction with the uranyl ion is the rate-determining step in the reaction.
Verification example 4
The intensity of light from the xenon lamp light source of example 1 was varied (15 mW/cm each) 2 、10mW/cm 2 、5mW/cm 2 ). As a result, as shown in fig. 8, it was found that the decrease in the uranyl ion concentration gradually slowed down with the decrease in the light intensity, and that less excited uranyl ions were generated.
Verification example 5
The amount of methanol added in example 1 was changed (0 mL and 0.1mL, respectively). As shown in fig. 9, it can be seen that the uranyl ion concentration does not decrease when methanol is not present, but the decrease tendency of uranyl ion gradually increases with the increase of the amount of methanol, indicating that methanol is an essential sacrificial agent for this process. The reason is that excited uranyl ions can abstract H element on methanol to generate free radicals.
The results of H-NMR measurements before and after the photocatalytic reaction of methanol show in FIG. 10 that the decrease of C-H bonds is observed, which indicates that C-H bonds in methanol are destroyed by the excited uranyl ions which deprive H elements on methanol. The specific reaction scheme is shown in FIG. 11.
The free radicals formed will continue to react, with (H-UO) 2 2+ ) Free radicals, which are unstable by themselves, are rapidly cleaved to H + And UO 2 + In the presence of oxygen, UO 2 + Oxidized to uranyl ion UO 2 2+ . And. CH 2 The OH radicals react with oxygen to form OOH radicals, which further react to form hydrogen peroxide. Under the condition of nitrogen, (H-UO) 2 2+ ) UO generated after radical cleavage 2 + Will directly react with CH 2 OH radical generation by reactionTo uranium dioxide and formaldehyde. Overall reaction scheme 12 shows the following equation:
·CH 2 OH+O 2 →·OOH+CH 2 O
OOH+·CH 2 OH→CH 2 O+H 2 O 2
verification example 6
By adding various actinide ions and alkali metal ions (actinide ions and alkali metal ions are Na) to uranyl nitrate solution + ，Ca 2+ ，Sr 2+ ，Cs + ，Co 2+ ，Ni 2+ ，La 3+ ，Ce 4+ ，Nd 3+ And the concentration is 0.4 mM), simulating radioactive wastewater, and performing selective extraction experiment of uranium by using a photocatalytic technology under the condition of no additional catalyst, wherein the result is shown in figure 13, and the result shows that the selectivity of the invention to uranium reaches more than 88%, and the removal rate of other coexisting ions is lower than 5%. The result shows that only the photochemical performance of the uranyl ions can carry out photochemical reaction with methanol under the condition of no additional catalyst, so that the solidification effect of the uranyl ions is realized, and the method has excellent selectivity.
The above description is only for the preferred embodiment of the present invention, and the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. A method for removing uranium by photocatalysis without a catalyst is characterized by comprising the following steps of adding organic matters into uranium-containing wastewater, mixing and stirring the organic matters and the wastewater, and then carrying out photocatalytic reaction.
2. A photocatalysis uranium removal method without a catalyst is characterized by comprising the following steps of adding hydrogen peroxide into uranium-containing wastewater, mixing and stirring the hydrogen peroxide and the uranium-containing wastewater, and reacting the hydrogen peroxide and the uranium-containing wastewater.
3. The method according to claim 1 or 2, characterized in that the uranium-bearing wastewater is wastewater containing uranyl ions, the wastewater containing uranyl ions has a pH value of 1 to 10, and the concentration of uranyl ions is 0.05 to 1mM.
4. The method of claim 1 or 2, wherein the organic is an alcohol organic; the volume ratio of the organic matter to the uranium-containing wastewater is (0.1-10): 50.
5. the method of claim 4, wherein the alcoholic organics comprise methanol, ethanol.
6. The method according to claim 1, wherein the photocatalytic reaction is carried out under an atmosphere of air and/or nitrogen gas and the light source used is a xenon lamp light source.
7. The method according to claim 5, wherein the xenon lamp light source has a full spectrum and an intensity of 0-50 mW/cm 2 。
8. The method according to claim 2, wherein the reaction is carried out under an air atmosphere, and the volume ratio of the hydrogen peroxide to the uranium-containing wastewater is (1-10): (10 to 100).
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