CN110127762B - Method for recycling uranium oxide from uranium-containing wastewater - Google Patents
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Abstract
The invention relates to a method for recycling uranium oxide from uranium-bearing waste water, which synthesizes polystyrene functional microspheres with abundant aldehyde groups on the surfaces in a copolymerization mode, then the microspheres are used for treating the uranium-bearing waste water, and the aldehyde groups on the surfaces of the microspheres provide binding sites to adsorb free uranyl ions (UO)2 2+) Oxidizing the microspheres by oxygen in the system, and finally obtaining the uranium oxide enriched polystyrene aldehyde microspheres. And (3) carrying out a burning method or an organic purification method on the prepared composite microspheres to obtain yellow uranium oxide recycled solid powder. Characterization was performed by infrared spectroscopy (FT-IR), Transmission Electron Microscopy (TEM), ultraviolet/visible spectrophotometer (UV-VIS), X-ray photoelectron spectroscopy (XPS). The recycling method for recycling uranium oxide from uranium-containing wastewater is simple in treatment process, mild in condition and strong in repeatability.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a method for recycling uranium oxide during uranium-containing wastewater treatment.
Background
China's republic of ChinaThe traditional energy development mainly comprises coal and petroleum, and with the technological progress and the appeal of people to green energy, the development and construction of nuclear energy are concerned more and more. Meanwhile, the treatment mode of radioactive wastewater generated in the development process of nuclear energy is also more and more emphasized. The waste water contains radioactive elements such as uranium, radium, cesium and the like, which pose great threats to the production and life safety of people. Of which uranium is the most common radioactive element, and which is generally in the hexavalent form (UO)2 2+) The main harm is ionization caused by radiation energy absorption, and easily induces cancer and other radioactive diseases, thus harming body health. Discharge of uranium-bearing wastewater into the environment can cause water pollution, death of vegetation and damage of ecological system balance.
The traditional technology for treating uranium-containing wastewater mainly comprises an ion exchange method, a membrane separation method, a biological method, an adsorption method and the like. The ion exchange method utilizes the difference of exchange capacity between exchangeable groups in the exchanger and different ions in the solution to carry out separation, has the advantages of higher removal rate and mature technology, and is also the most widely applied in the nuclear wastewater treatment at present. But the influence of interfering ions is large, the operating conditions are harsh, and the price of the ion exchange resin is expensive. The membrane separation technology utilizes a semipermeable membrane with selective permeability, takes external pressure (such as pressure difference, concentration difference, potential difference and the like) as driving force, and selectively permeates components in a mixed solution, thereby achieving the purposes of separation, classification, purification and concentration. The membrane separation technology has the advantages of no phase change of materials, low energy consumption, simple and convenient operation, low equipment requirement, good separation effect, no secondary pollution, energy conservation, environmental protection and the like. However, permselective membranes are expensive and are prone to membrane fouling during processing, which limits the usefulness of the methods and processes. The bioadsorption is mainly based on microorganisms in nature, including bacteria, fungi and algae, and various agricultural wastes and biomass, and has wide sources, low cost and easy availability, but has low efficiency and is difficult to industrialize.
Disclosure of Invention
Aiming at the defects of various methods for treating uranium-containing wastewater in the prior art, the invention provides a novel method for treating uranium-containing wastewater and recovering uranium oxide from the uranium-containing wastewater.
The invention aims to realize the recycling method of recycling uranium oxide in uranium-containing wastewater, and is characterized by comprising the following steps:
1) taking azodiisobutyronitrile as an initiator, polyvinylpyrrolidone as a dispersant, and isopropanol and water as solvents, and taking styrene and acrolein as monomers to perform copolymerization reaction to prepare monodisperse polystyrene aldehyde microspheres;
2) dissolving the polystyrene aldehyde microspheres in a mixed solution of isopropanol and/or water according to the proportion of 0.01-0.012 g/mL, uniformly mixing the mixed solution with uranium-containing wastewater, stirring the mixed solution for reaction for 2-4 h under the condition of a constant-temperature water bath at 65-70 ℃, separating the microspheres and liquid from the reacted product through high-speed centrifugal sedimentation, washing the suspended microspheres through deionized water ultrasonic centrifugation, and drying the microspheres for 48-72 h at 55-65 ℃ to obtain the polystyrene aldehyde microspheres enriched with uranium oxide;
3) and recycling the uranium oxide in the uranium oxide-enriched polystyrene aldehyde-based microspheres by a burning method or an organic matter extraction method.
The method for treating the uranium-containing wastewater synthesizes polystyrene functional microspheres with abundant aldehyde groups on the surfaces in a copolymerization mode, wherein the aldehyde groups provide binding sites for adsorbing uranyl ions (UO) in the wastewater2 2+) Oxidizing the microspheres by oxygen in the system to finally obtain the uranium oxide-enriched polystyrene aldehyde microspheres, and obtaining the uranium oxide (U) by a burning method or an organic matter extraction method3O8) Recovering the product. Compared with the prior art, the method has the following advantages:
1. the process flow is simple, and uranyl ions can be enriched on the surfaces of the microspheres only by mixing the polystyrene aldehyde-based spheres with uranium-containing wastewater and stirring for reaction at the temperature of 70 ℃ in a constant-temperature water bath;
2. the polystyrene microspheres are convenient to recover, and can be separated and recovered by proper heating due to low melting point and full combustion at high temperature;
3. convenient detection, uranyl ion (UO)2 2+) Can form a stable complex with the azo arsine-III under the acidic condition. The absorbance of the solution at a specific absorption wavelength can be measured by an ultraviolet/visible spectrophotometer, so that the change of the solution concentration before and after adsorption and the adsorption rate can be calculated.
In the invention, the preparation of the monodisperse polystyrene-based microspheres comprises the following steps:
1.1) dissolving polyvinylpyrrolidone in an equal volume of mixed aqueous isopropanol solution to obtain a concentration of: 0.12 g-0.15 g/mL polyvinylpyrrolidone solution;
1.2) dissolving an initiator azobisisobutyronitrile into styrene to prepare a styrene solution dissolved with the initiator, wherein the proportion of the azobisisobutyronitrile to the styrene is 0.012 g-0.018 g/mL;
1.3) mixing the polyvinylpyrrolidone solution obtained in the step 1.1) with the styrene solution obtained in the step 1.2), fully stirring for 30min, adding a proper amount of acrolein, wherein the volume of the acrolein is 0.5-1 time of that of styrene, reacting for 8 h in a water bath at 70 ℃ after mixing, and centrifugally separating, washing and drying the suspension generated by the reaction to obtain the polystyrene aldehyde group microspheres.
In order to improve the adsorption capacity of the microspheres to uranyl ions, in the step 2), after the treatment liquid is mixed with uranium-containing wastewater, the pH value of the mixed liquid is adjusted to 7-8 through ammonia water.
In order to ensure the safe discharge of the waste water after adsorption, in the step 2), the liquid separated by the mixed liquid after adsorption reaction is subjected to high-speed centrifugal sedimentation and is subjected to membrane filtration treatment before being discharged.
Preferably, in step 3), the method for recovering uranium oxide by a burning method comprises the following steps: putting the uranium oxide-enriched polystyrene aldehyde group microsphere powder into a crucible, heating the powder in a heating furnace platform to 180-220 ℃, preserving the heat for 2-3 h, naturally cooling, taking out the residual yellow solid at the bottom, repeatedly cleaning the solid with ethanol or aqueous solution, and drying the solid for 24-30 h at 55-65 DEG Ch obtaining the recycled uranium oxide (U)3O8）。
Preferably, in step 3), the organic matter extraction method comprises: dissolving the polystyrene aldehyde group microsphere powder enriched with uranium oxide in 20mL of N, N-dimethyl formyl solution, preparing a mixed solution with the concentration of 0.006 g-0.008 g/mL, performing ultrasonic-assisted dissolution, stirring for 2 h-3 h at 20-25 ℃, centrifugally separating out yellow solid at the bottom, washing with ethanol or aqueous solution for multiple times, and drying for 24 h-30 h at 55-65 ℃ to obtain the recovered uranium oxide.
Drawings
FIG. 1 is a representation of an infrared spectrum of polystyrene-based microspheres of the present invention.
FIG. 2a is a transmission electron microscopy characterization of polystyrene-based microspheres of the present invention.
FIG. 2b is a transmission electron microscope characterization chart of the polystyrene-based microspheres with an adsorption concentration of 5ppm uranium acetate.
FIG. 2c is a transmission electron microscope characterization chart of the polystyrene-based microspheres with the adsorption concentration of 10ppm uranium acetate.
FIG. 2d is a transmission electron microscope characterization chart of the polystyrene-based microspheres with an adsorption concentration of 50ppm uranium acetate.
FIG. 3a is a graph of the ultraviolet spectrum of a uranium acetate solution at concentrations of 0, 5ppm, 10ppm, and 50ppm before adsorption.
FIG. 3b is a graph showing the UV spectra of uranium acetate solutions having concentrations of 5ppm, 10ppm, and 50ppm, respectively, after adsorption.
FIG. 4 shows uranium oxide (U)3O8) An X-ray photoelectron spectroscopy characterization map.
Detailed Description
Example 1
Firstly, preparing polystyrene aldehyde group microspheres:
(1) mixing 18 mL of isopropanol and 2.5 g of polyvinylpyrrolidone PVP dispersing agent, adding the mixture into a three-neck flask with a condensing tube after ultrasonic-assisted dissolution, placing the three-neck flask into a constant-temperature water bath kettle at 70 ℃, and mechanically stirring and keeping the rotating speed at 315 r/min;
(2) dissolving 0.1g of Azobisisobutyronitrile (AIBN) initiator into 6mL of styrene to prepare a styrene solution dissolved with the initiator;
(3) adding the styrene solution (2) dissolved with the initiator into the system obtained in (1), stirring to fully mix for 30min, and adding 3 mL of acrolein C3H4And O, reacting for 8 hours at a constant temperature of 70 ℃, after the reaction is stopped, ultrasonically centrifuging and washing for three times by using ethanol and water to prepare polystyrene aldehyde group ball emulsion, and drying to obtain the polystyrene aldehyde group microspheres.
Then, adsorbing uranyl ions by using the polystyrene aldehyde group PS-CHO microspheres:
simulating uranium-containing wastewater by using a uranium acetate aqueous solution, and respectively preparing appropriate uranium acetate aqueous solutions with the concentrations of 5ppm, 10ppm and 50ppm for simulating wastewater with different uranium contents; respectively dissolving 0.2g of the prepared polystyrene aldehyde group microspheres in 20mL of isopropanol solution, respectively pouring the obtained mixture into four 150mL three-neck flasks after ultrasonic-assisted dissolution, wherein the numbers of the flasks are 1, 2, 3 and 4, respectively dripping 100mL of uranium acetate aqueous solution with the concentrations of 5ppm, 10ppm and 50ppm from the three-neck flasks 2, 3 and 4 at the rotating speed of 315r/min, adjusting the pH value to be =7.5 by using ammonia water, reacting for two hours in a constant-temperature water bath at 70 ℃, stopping the reaction, separating suspended microspheres from the reacted mixed solution by high-speed centrifugal sedimentation, respectively washing the suspended microspheres by ultrasonic centrifugation with ethanol and water, and drying for 48 to 72 hours at the temperature of 55 to 65 ℃ to obtain the polystyrene aldehyde group microsphere powder enriched with uranium oxide. Meanwhile, the liquid separated from the No. 2, No. 3 and No. 4 three-neck flasks is filtered through a membrane filter with the filter pore diameter of 22 mu m to further filter out the non-settled microspheres, and each separated liquid is respectively reserved for detecting the uranium content in the liquid.
And finally, recycling uranium oxide, in the embodiment, the polystyrene aldehyde group microsphere powder which is separated and cleaned from No. 2 and No. 3 three-neck flasks and is enriched with uranium oxide is respectively placed in a crucible, then the crucible is placed in a muffle furnace to be heated for 2 hours at 200 ℃, the residual yellow solid at the bottom is taken out after the polystyrene aldehyde group microsphere powder is naturally cooled, the mixed solution of ethanol and water is used for cleaning for more than 3 times, and the mixed solution is dried for 24 hours at 60 ℃ to obtain the solid uranium oxide.
In addition, dissolving the corresponding uranium oxide-enriched polystyrene aldehyde group microsphere powder of the No. 4 three-neck flask in 20mL of N, N-dimethyl formyl (DMF) solution, wherein the proportion of the microspheres to the solution is 0.010 g/mL, performing ultrasonic-assisted dissolution, stirring for 2 h at 25 ℃, centrifugally separating out yellow solid at the bottom, washing for multiple times by using a mixed solution of ethanol and water, and drying for 24 h at 60 ℃ to obtain the solid uranium oxide.
Analytical examples
This example was conducted to analytically verify the components prepared in example 1.
Firstly, mixing the polystyrene aldehyde group microspheres prepared in the embodiment with potassium bromide according to the proportion of 1:100, and drying under an ultraviolet lamp. Grinding into fine powder in a mortar, tabletting under a pressure of 5MPa, and characterizing by a Fourier infrared spectrometer as shown in FIG. 1 at 3100 and 2800cm-1Four peaks at are all from sp of benzene ring2C-H stretching vibration; at 1499cm-1And 1455cm-1The peak of (A) belongs to sp of a benzene ring skeleton (-C = C-)2C-H stretching vibration; the C-H deformation vibration peak of the monosubstituted benzene is 1029cm-1And 753cm-1At least one of (1) and (b); 1724cm-1C = O absorption peak and 2706cm of aldehyde group at (2)-1C-H absorption peak of aldehyde group shows that styrene and acrolein have copolymerization reaction, and the aldehyde group is fixed on the surface of the microsphere.
As shown in fig. 2, wherein fig. 2a is a transmission electron microscopy characterization image of polystyrene-based microspheres;
FIG. 2b is a transmission electron microscope image of the uranium oxide-enriched polystyrene aldehyde microspheres adsorbing 5ppm of uranium acetate;
FIG. 2c is a transmission electron microscope image of the uranium oxide-enriched polystyrene aldehyde microspheres adsorbing 10ppm of uranium acetate;
FIG. 2d is a transmission electron micrograph of uranium oxide-enriched polystyrene aldehyde microspheres adsorbing 50ppm of uranium acetate.
It is obvious from the electron microscope images of the figures that the surface of the polystyrene aldehyde microsphere is fixed with micro uranium milling groups or uranium oxide particles to different degrees.
In order to verify whether uranyl ions in the adsorbed uranium acetate solution are adsorbed and removed by polystyrene microspheres, the solutions before and after adsorption in three-necked flasks No. 2, No. 3 and No. 4 in example 1 are subjected to membrane filtration, and the filtered solutions are respectively mixed with a color developing agent according to a volume ratio of 1: 3 mixing, and measuring the absorbance of the solution by a spectrophotometer to detect whether the uranyl ions in the solution are reduced to the concentration meeting the emission standard.
The color developing agent is prepared in advance according to the following method, 0.07g of arsine-III powder is dissolved in 100mL of perchloric acid solution with the concentration of 3 mol/L, ultrasonic-assisted dissolution is carried out, and the color developing agent solution can be obtained after standing for one week. The solution and the color developing agent are mixed according to the volume ratio of 1: 3, and the absorbance of the mixture is measured by ultraviolet/visible spectrophotometry. The uv spectra of the solutions with uranium concentrations of 5, 10 and 50ppm, respectively, as shown in fig. 3a, show that the uranyl ion has an absorption peak at the characteristic absorption wavelength of 651 nm. According to a calculation formula of the change rate of the concentration of the uranyl ions:
C0: initial concentration (ppm); cE: equilibrium concentration (ppm)
When the concentration of the uranyl ions in the solution is less than 10ppm, after two hours of adsorption, an absorption peak disappears at 651nm, and the residual uranyl ions in the solution are proved to be lower than the detection limit of an ultraviolet/visible spectrophotometer. When the concentration was increased to 50ppm, the adsorption rate reached 83.57%. Therefore, the polystyrene aldehyde group microsphere has strong adsorption capacity and good adsorption effect on the solution containing the uranyl ions.
As shown in fig. 4, which is a graph representing the X-ray photoelectron spectrum of the uranium oxide recovered in example 1, XPS U4f spectrum of the uranium oxide shows that the U4f 5/2 and U4f 7/2 binding energies are 392.6 eV and 381.7 eV, respectively. The characterization results were consistent with previous findings. However, satellite peaks are observed at the high binding energy ends of U4f 5/2 and U4f 7/2, so that the conclusion that U is high can be inferred3O8Is UO2And UO3A composite of components.
Therefore, the method for recycling uranium oxide in uranium-containing wastewater treatment synthesizes polystyrene with abundant aldehyde groups on the surface in a copolymerization modeCan provide binding sites for microspheres and aldehyde groups to adsorb uranyl ions (UO) in wastewater2 2+) Oxidizing the microspheres by oxygen in the system to finally obtain the uranium oxide-enriched polystyrene aldehyde microspheres, and obtaining the uranium oxide (U) by a burning method or an organic matter extraction method3O8）The recovered substance has the advantages of simple process flow, convenient recovery operation, convenient detection means and convenient emission control in industrial application.
Claims (6)
1. A method for recycling uranium oxide from uranium-containing wastewater is characterized by comprising the following steps:
step 1) taking azobisisobutyronitrile as an initiator, polyvinylpyrrolidone as a dispersant and isopropanol and water as solvents, and taking styrene and acrolein as monomers to perform copolymerization reaction to prepare monodisperse polystyrene aldehyde group microsphere floating liquid;
step 2) dissolving the polystyrene aldehyde microspheres in a mixed solution of isopropanol and/or water according to the proportion of 0.01-0.012 g/mL, uniformly mixing the mixed solution with uranium-containing wastewater according to the proportion of 0.002-0.0025 g/mL, stirring and reacting for 2-4 h under the condition of a constant-temperature water bath at 65-70 ℃, separating the microspheres and liquid from the reacted product through high-speed centrifugal sedimentation, ultrasonically and centrifugally washing the suspended microspheres with deionized water, and drying for 48-72 h at 55-65 ℃ to obtain the uranium oxide-enriched polystyrene aldehyde microspheres;
and 3) recovering uranium oxide in the uranium oxide-enriched polystyrene aldehyde-based microspheres by a burning method or an organic matter extraction method.
2. The method for recovering uranium oxide from uranium-containing wastewater according to claim 1, wherein the step 1) of preparing monodisperse polystyrene-based microspheres comprises the following steps:
1.1) dissolving polyvinylpyrrolidone in an equal volume of mixed aqueous isopropanol solution to obtain a concentration of: 0.12 g-0.15 g/mL polyvinylpyrrolidone solution;
1.2) dissolving an initiator azobisisobutyronitrile into styrene to prepare a styrene solution dissolved with the initiator, wherein the proportion of the azobisisobutyronitrile to the styrene is 0.012 g-0.018 g/mL;
1.3) mixing the polyvinylpyrrolidone solution obtained in the step 1.1) with the styrene solution obtained in the step 1.2), fully stirring for 30min, adding a proper amount of acrolein, wherein the volume of the acrolein is 0.5-1 time of that of styrene, reacting for 8 h in a water bath at 70 ℃ after mixing, and centrifugally separating, washing and drying the suspension generated by the reaction to obtain the polystyrene aldehyde group microspheres.
3. The method for recycling uranium oxide from uranium-containing wastewater according to claim 1, wherein in the step 2), after the treatment liquid is mixed with the uranium-containing wastewater, the pH value of the mixed liquid is adjusted to 7-8 by ammonia water.
4. The method for recovering uranium oxide from uranium-containing wastewater according to claim 1, wherein in the step 2), the liquid separated by high-speed centrifugal sedimentation of the mixed liquid after adsorption reaction is treated by membrane filtration before discharge.
5. The method for recycling uranium oxide from uranium-containing wastewater according to claim 1, wherein in the step 3), the method for recycling uranium oxide by a burning method comprises the following steps: putting the uranium oxide-enriched polystyrene aldehyde group microsphere powder into a crucible, heating the powder in a heating furnace platform to 180-220 ℃, preserving the heat for 2-3 h, naturally cooling, taking out the residual yellow solid at the bottom, repeatedly cleaning the solid with ethanol or aqueous solution, and drying the solid for 24-30 h at 55-65 ℃ to obtain the recycled uranium oxide.
6. The method for recycling uranium oxide from uranium-containing wastewater according to claim 1, wherein in the step 3), the organic matter extraction method comprises: dissolving the polystyrene aldehyde group microsphere powder enriched with uranium oxide in 20mL of N, N-dimethyl formyl solution, preparing a mixed solution with the concentration of 0.006 g-0.008 g/mL, performing ultrasonic-assisted dissolution, stirring for 2 h-3 h at 20-25 ℃, centrifugally separating out yellow solid at the bottom, washing with ethanol or aqueous solution for multiple times, and drying for 24 h-30 h at 55-65 ℃ to obtain the recovered uranium oxide.
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