CN114496331A - Method for efficiently reducing uranyl - Google Patents

Method for efficiently reducing uranyl Download PDF

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CN114496331A
CN114496331A CN202111638562.5A CN202111638562A CN114496331A CN 114496331 A CN114496331 A CN 114496331A CN 202111638562 A CN202111638562 A CN 202111638562A CN 114496331 A CN114496331 A CN 114496331A
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uranyl
benzyl alcohol
supernatant
under
benzaldehyde
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王宏青
李跃欢
史浪
孙群英
刘灿
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University of South China
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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
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24—Nitrogen compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G43/00—Compounds of uranium
    • C01G43/01—Oxides; Hydroxides
    • C01G43/025—Uranium dioxide
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
    • C07C45/38—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
    • 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
    • G21F9/20—Disposal of liquid waste

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Abstract

The invention discloses a method for efficiently reducing uranyl, which belongs to the technical field of chemical engineering, and comprises the steps of firstly preparing a catalyst, and then adding a photocatalyst and benzyl alcohol into UO2 under a xenon lamp provided with a 420 nm cut-off filter2+Stirring the solution in the dark for two hours to reach adsorption-desorption balance, then carrying out illumination, taking supernatant after illumination, filtering the supernatant by using a syringe filter, and analyzing the concentrations of uranyl, benzyl alcohol and benzaldehyde; the oxidation of the benzyl alcohol needs the participation of oxygen, and the oxygen and UO2 are reduced2+Compete for electrons, thereby improving the reduction of UO2 under aerobic conditions2+Meanwhile, the oxidation of the benzyl alcohol is carried out in the presence of oxygen, so that the benzaldehyde with economic value is finally generated, and the oxidation of the benzyl alcohol is promoted under the aerobic condition, so that the reduction of the uranyl is accelerated.

Description

Method for efficiently reducing uranyl
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method for efficiently reducing uranyl.
Background
With the rapid development of the nuclear industry, a large amount of uranium pollutants are released into a water environment, and great harm is caused to the environment and human bodies. Therefore, it is necessary to deal with the uranium contamination problem. Uranium has four chemical forms: u (III), U (IV), U (V) and U (VI), wherein the soluble U (VI) and the insoluble U (IV) are the most stable. U (VI) is easily dissolved in the environment and easily diffused in the environment, thus causing more serious environmental pollution. In contrast, u (iv) is insoluble in the environment, does not readily diffuse, and is less harmful to the environment. At present, methods for treating uranium-containing wastewater mainly comprise an adsorption method and an ion exchange method. Although these processes are simple and effective, they are still adsorbed on the material in the form of U (VI) and separated from the wastewater. During desorption or work-up, it is still possible to release u (vi) into the environment and migrate with the water. Meanwhile, the treated materials may cause secondary pollution. Therefore, reduction of soluble u (vi) to insoluble u (iv) to prevent u (vi) migration with water is considered a more reliable and effective strategy for removing uranyl contamination. In recent years, the photocatalytic reduction method has attracted much attention because of its advantages of high efficiency, high solar energy utilization rate, no secondary pollution, reusability, relatively low cost, etc. Thus, the conversion of soluble u (vi) to insoluble u (iv) in aqueous solution becomes a hotspot followed by photocatalytic reduction.
Currently, most photocatalytic systems achieve the reduction of UO22+ to UO2 in the absence of oxygen, primarily because oxygen will first combine with photogenerated electrons under aerobic conditions, making it difficult for UO22+ to gain electrons. Lu et al reported that the photocatalytic reduction efficiency of B-g-C3N4 for UO22+ decreased by 23% when the nitrogen atmosphere was replaced with oxygen. However, uranium-containing wastewater typically contains oxygen. Moreover, even if nitrogen is continuously introduced into the system to eliminate the influence of oxygen, the process is also more complicated, and the cost in the treatment process is increased. Although there is such a report on u (vi) photoreduction in aqueous solution in the presence of oxygen, there is no mention or solution that aerobic conditions are more effective than anaerobic conditions in reducing uranyl, and that the catalyst SnO2/CdCO3/cds (scc) nanocomposites are corroded and cannot be reused. In addition, the photocatalytic reduction of uranyl is not only oxygen-free, but also adds some organic matters as sacrificial agents, only used for consuming cavities and wasted by the cavity oxidation. Unfortunately, the process fails to synergistically reduce uranyl and oxidized organics for the purposes of fixing uranium and preparing other organics. There is an urgent need to find a method for preparing valuable organic substances by synergistically reducing UO22+ and holes by making full use of electrons under aerobic conditions.
In principle, after exposure of the catalyst to light, electrons present in the conduction band participate in the uranyl reduction reaction, while holes in the valence band participate in the oxidation reaction of the organic substrate. It can be concluded from this that if dissolved oxygen is more likely to participate in the oxidation process of organic matter, it will not compete with uranyl for photogenerated electrons. In other words, whether oxygen participates in the mechanism for oxidizing organic matter will affect whether the photocatalytic reduction of uranyl can be carried out under aerobic conditions. The key to solving the problem is to construct a coupled catalytic system by screening target objects from potential organic substrates.
Recent studies have shown that photogenerated holes and oxygen play a crucial role in the photocatalytic oxidation of aromatic alcohols to aromatic aldehydes. Zhao et al disclose that the oxygen atom in the alcohol-converted aldehyde is derived from the oxygen atom in dissolved oxygen, indicating that oxygen is involved in the oxidation reaction of the alcohol to the aldehyde. Therefore, the aromatic alcohol can fully utilize oxygen and a cavity to generate valuable aromatic aldehyde, simultaneously reduces competition of oxygen and uranyl ions for electrons, and provides a feasible solution for reducing uranyl under aerobic conditions.
Disclosure of Invention
The invention aims to provide a method for efficiently reducing uranyl.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a method for efficiently reducing uranyl comprises the following steps:
the catalyst was prepared first and then the photocatalyst and benzyl alcohol were added to UO2 under a xenon lamp equipped with a 420 nm cut-off filter2+Stirring in dark for two hours to reach adsorption-desorption equilibrium, and irradiating with lightAnd taking the supernatant, filtering the supernatant by using a syringe filter, and analyzing the concentrations of uranyl, benzyl alcohol and benzaldehyde.
As a further scheme of the invention: the photocatalyst is one of B-CN, K-CN, Na-CN and NaK-CN.
As a further scheme of the invention: the method comprises the following steps:
firstly preparing a catalyst, and then adding 5-50mg of the photocatalyst and 0.1-3ml of benzyl alcohol to 50 ml of 20 mg/L UO2 under a xenon lamp equipped with a 420 nm cut-off filter2+Stirring the solution in the dark for two hours to reach adsorption-desorption equilibrium, then irradiating with light, taking the supernatant after the light irradiation, filtering the supernatant with a syringe filter, and analyzing the concentrations of uranyl, benzyl alcohol and benzaldehyde.
As a further scheme of the invention: the benzyl alcohol is added to UO2 under oxygen-free conditions2+In solution.
As a further scheme of the invention: the benzyl alcohol is added to UO2 under aerobic conditions2+In solution.
As a further scheme of the invention: the preparation method of NaK-CN comprises the following steps:
respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product named as NaK-CN.
As a further scheme of the invention: the uranyl concentration is measured at 652 nm by an ultraviolet-visible spectrophotometer, and the adopted color developing agent is azoarsenIII; the benzyl alcohol and benzaldehyde concentrations were analyzed by high performance liquid chromatography.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a method for efficiently reducing uranyl, wherein the oxidation of benzyl alcohol needs the participation of oxygen, and the oxygen and UO2 are reduced2+Compete for electrons, thereby improving the reduction of UO2 under aerobic conditions2+The oxidation of the benzyl alcohol is not needed, meanwhile, the oxidation of the benzyl alcohol is carried out in the presence of oxygen, so that the benzaldehyde with economic value is finally generated, and the oxidation of the benzyl alcohol is promoted under the aerobic condition, so that the oxidation of the benzyl alcohol is acceleratedReduction of uranyl is performed.
Drawings
FIG. 1 shows UO2 on photocatalysts of B-CN, NaK-CN, K-CN and Na-CN2+Concentration as a function of irradiation time.
FIG. 2 shows UO2 of NaK-CN photocatalyst with N2, air and/or methanol, benzyl alcohol2+Concentration as a function of irradiation time.
FIG. 3 is a graph showing the HPLC analysis of the concentrations of benzyl alcohol and benzaldehyde in example 1.
Detailed Description
Example 1
Preparation of sodium-potassium co-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product, thus obtaining the sodium-potassium co-doped carbon nitride, which is named as NaK-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, under the aerobic condition, 5-50mg NaK-CN and 0.1-3ml benzyl alcohol are added into 50 ml 20 mg/L UO22+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, and the uranyl concentration was measured at 652 nm by an ultraviolet-visible spectrophotometer using azoarsenic iii as a color developing agent, and as shown in fig. 1 and 2, the concentrations of benzyl alcohol and benzaldehyde were analyzed by high performance liquid chromatography, and the results are shown in fig. 3.
Example 2
Preparing sodium potassium single-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride or 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 500-580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product named as K-CN/Na-CN.
Under the condition of aerobic condition, adding 5-50mgK-CN and 0.1-3ml benzyl alcohol into 50 ml 20 mg/L UO2 under a xenon lamp equipped with 420 nm cut-off filter2+In the solution, the photocatalysis experiment is carried out, and before the irradiation, the reaction system is in the darkAfter stirring for two hours to reach adsorption-desorption equilibrium, and light irradiation for 10 to 120 minutes, 1 mL of the supernatant was taken, filtered with a 0.45 μm syringe filter, and analyzed for uranyl, benzyl alcohol, and benzaldehyde concentrations, as measured by an ultraviolet-visible spectrophotometer at 652 nm, using azo arsenic III as a color developing agent, and the results are shown in FIG. 1.
Example 3
Preparing sodium potassium single-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride or 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product named as K-CN/Na-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, under aerobic conditions, 5-50mg of Na-CN and 0.1-3ml of benzyl alcohol are added into 50 ml of 20 mg/L UO22+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, the uranyl concentration was measured by an ultraviolet-visible spectrophotometer at 652 nm, and the color-developing agent used was azoarsenium iii, the results of which are shown in fig. 1.
Example 4
Preparing pure carbon nitride: adding melamine into the crucible, calcining for 2-4 hours in a muffle furnace at the temperature of 500-580 ℃, cooling, washing and drying to obtain a product named as B-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, 5-50mgB-CN and 0.1-3ml benzyl alcohol are added into 50 ml 20 mg/L UO2 under the aerobic condition2+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, the uranyl concentration was measured by an ultraviolet-visible spectrophotometer at 652 nm, and the color-developing agent used was azoarsenium iii, the results of which are shown in fig. 1.
Example 5
Preparation of sodium-potassium co-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product, thus obtaining the sodium-potassium co-doped carbon nitride, which is named as NaK-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, under the aerobic condition, 5-50mg NaK-CN and 0.1-3ml methanol are added into 50 ml 20 mg/L UO22+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, the uranyl concentration was measured by an ultraviolet-visible spectrophotometer at 652 nm, and the color-developing agent used was azoarsenium iii, the results of which are shown in fig. 2.
Example 6
Preparation of sodium-potassium co-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product, thus obtaining the sodium-potassium co-doped carbon nitride, which is named as NaK-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, under the aerobic condition, 5-50mg NaK-CN and 0.1-3ml benzyl alcohol are added into 50 ml 20 mg/L UO22+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, the uranyl concentration was measured by an ultraviolet-visible spectrophotometer at 652 nm, and the color-developing agent used was azoarsenium iii, the results of which are shown in fig. 2.
Example 7
Preparation of sodium-potassium co-doped carbon nitride: respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product, thus obtaining the sodium-potassium co-doped carbon nitride, which is named as NaK-CN.
Under a xenon lamp equipped with a 420 nm cut-off filter, under nitrogenUnder the condition of adding 5-50mg of NaK-CN and 0.1-3ml of methanol into 50 ml of 20 mg/L UO22+In the solution, a photocatalytic experiment was performed, and before irradiation, the reaction system was stirred in the dark for two hours to reach an adsorption-desorption equilibrium, and after 10 to 120 minutes of irradiation, 1 mL of the supernatant was taken and filtered with a 0.45 μm syringe filter to analyze the concentrations of uranyl, benzyl alcohol and benzaldehyde, the uranyl concentration was measured by an ultraviolet-visible spectrophotometer at 652 nm, and the color-developing agent used was azoarsenium iii, the results of which are shown in fig. 2.
In summary, the following steps: as can be seen from fig. 1, the sodium-potassium double-doped carbon nitride has a much stronger ability to reduce uranyl than sodium or potassium single-doped carbon nitride. As can be seen from FIG. 2, when methanol was introduced as an organic substrate under aerobic conditions, NaK-CN photocatalyst pairs UO2 were observed after 20 minutes of visible light irradiation2+The reduction ratio of (2) was only 62%, whereas when benzyl alcohol was introduced, a reduction ratio of nearly 100% was achieved. The main reason for this difference is that the oxidation of benzyl alcohol requires the participation of oxygen, which is reduced from UO22+Compete for electrons, thereby increasing the reduction of UO2 under aerobic conditions2+While oxidation of methanol is not required. Meanwhile, the oxidation of the benzyl alcohol is carried out in the presence of oxygen, and finally, benzaldehyde with economic value is generated. In addition, the difference of introducing benzyl alcohol to reduce uranyl under the aerobic and anaerobic conditions is also explored. As can be seen from fig. 1, the reduction rate of uranyl under aerobic conditions is faster than under anaerobic conditions. This demonstrates that oxygen promotes the oxidation of benzyl alcohol, which in turn accelerates the reduction of uranyl.

Claims (7)

1. The method for efficiently reducing uranyl is characterized by comprising the following steps:
the catalyst was prepared first and then the photocatalyst and benzyl alcohol were added to UO2 under a xenon lamp equipped with a 420 nm cut-off filter2+Stirring the solution in the dark for two hours to reach adsorption-desorption equilibrium, then irradiating with light, taking the supernatant after the light irradiation, filtering the supernatant with a syringe filter, and analyzing the concentrations of uranyl, benzyl alcohol and benzaldehyde.
2. The method for efficiently reducing uranyl according to claim 1, wherein the photocatalyst is one of B-CN, K-CN, Na-CN, and NaK-CN.
3. A process for efficient reduction of uranyl according to claim 1 including the steps of:
firstly preparing a catalyst, and then adding 5-50mg of the photocatalyst and 0.1-3ml of benzyl alcohol to 50 ml of 20 mg/L UO2 under a xenon lamp equipped with a 420 nm cut-off filter2+Stirring the solution in the dark for two hours to reach adsorption-desorption equilibrium, then irradiating with light, taking the supernatant after the light irradiation, filtering the supernatant with a syringe filter, and analyzing the concentrations of uranyl, benzyl alcohol and benzaldehyde.
4. The method for efficient reduction of uranyl according to claim 3 wherein said benzyl alcohol is added under oxygen-free conditions to UO22+In solution.
5. The method for efficient reduction of uranyl according to claim 3 wherein benzyl alcohol is added aerobically to UO22+In solution.
6. The method for efficiently reducing uranyl according to claim 3, wherein the NaK-CN is prepared by the following steps:
respectively adding a mixture of 1-10g of melamine, 1-20g of potassium chloride and 1-20g of sodium chloride into the crucible, calcining for 2-4 hours at the temperature of 580 ℃ in a muffle furnace, cooling, washing and drying to obtain a product named as NaK-CN.
7. A process for efficient reduction of uranyl according to claim 3 wherein the uranyl concentration is measured at 652 nm by an ultraviolet-visible spectrophotometer using azo arsenium iii as a color reagent; the benzyl alcohol and benzaldehyde concentrations were analyzed by high performance liquid chromatography.
CN202111638562.5A 2021-12-29 2021-12-29 Method for efficiently reducing uranyl Pending CN114496331A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115228500A (en) * 2022-08-11 2022-10-25 哈尔滨工程大学 High-dispersity C 3 N 4 Composite material for extracting uranium from seawater and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115228500A (en) * 2022-08-11 2022-10-25 哈尔滨工程大学 High-dispersity C 3 N 4 Composite material for extracting uranium from seawater and preparation method thereof

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