CN113582300A - Method for removing uranium element in water through electro-adsorption - Google Patents
Method for removing uranium element in water through electro-adsorption Download PDFInfo
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Abstract
The invention provides a method for removing uranium element in water by electro-adsorption, belonging to the technical field of water treatment. The invention takes carbon aerogel as raw material for electric adsorption, and the carbon aerogel is treated by CO2After thermal activation, the carbon nano-tube has rich mesoporous structure, increases the specific surface area and improves the adsorption effect in the electric adsorption process; the uranium element is removed by utilizing the electric adsorption, an electric field is formed between the electric adsorption modules in the electric adsorption process, uranium-containing water flows between the electric adsorption modules, uranium ions in the water move to the surface of the activated carbon aerogel electrode with opposite charges through the electric field force and are finally adsorbed in the pores of the activated carbon aerogel electrode, and therefore the total concentration of the uranium element in the water is reduced. The method provided by the invention is simple to operate, has low cost and is suitable for large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a method for removing uranium element in water through electro-adsorption.
Background
Uranium is a very common radioactive element, the heaviest element in nature, and is commonly found in groundwater from all over the world. The toxicity of uranium is determined by its chemical and radioactive properties. All uranium mixtures are considered toxic and may cause nephrotoxic effects. The presence of higher levels of uranium in the human body can affect kidney function and even lead to renal failure. The main mechanism of uranium access to the human body is through the ingestion of groundwater contaminated with radioactive waste.
At present, the method for removing uranium in water is mainly a reverse osmosis treatment method, and a used reverse osmosis system comprises a filter membrane, an activated carbon filter, a terminal carbon filter and the like, but the reverse osmosis treatment method is complex and has high cost, and is not suitable for large-scale popularization and application.
Disclosure of Invention
In view of the above, the present invention is directed to a method for removing uranium element from water by electro-adsorption. The method provided by the invention is simple to operate and low in cost, and can effectively remove uranium in water.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for removing uranium element in water by electric adsorption, which comprises the following steps:
(1) in CO2Thermally activating the carbon aerogel in the atmosphere to obtain activated carbon aerogel;
(2) and assembling the activated carbon aerogel into an electric adsorption module by taking the activated carbon aerogel as an electrode, and applying voltage on the electric adsorption module to enable the uranium-containing water to circularly pass through the electric adsorption module for electric adsorption.
Preferably, the temperature of the heat activation in the step (1) is 800-1000 ℃, and the time is 1.5-3 h.
Preferably, the specific surface area of the activated carbon aerogel is 1200-2000 cm2·g-1The total pore volume is 1.5-3 cm3·g-1。
Preferably, before the assembling, the method further comprises modifying the activated carbon aerogel, wherein the modifying comprises:
and ultrasonically mixing the activated carbon aerogel with a soluble divalent manganese salt and a potassium permanganate solution, and carrying out solid-liquid separation to obtain the manganese dioxide modified activated carbon aerogel.
Preferably, the mass ratio of the activated carbon aerogel to the soluble divalent manganese salt is 1: 0.15-0.4.
Preferably, the applied voltage is 0.8 to 1.4V.
Preferably, the content of uranium ions in the uranium-containing water is 10-200 mg/L.
Preferably, the speed of the uranium-containing water passing through the electric adsorption module is 10-25 mL/min.
Preferably, during the process of the electro-adsorption, the method further comprises monitoring the conductivity of the uranium-containing water during the electro-adsorption, and when the conductivity of the uranium-containing water is kept stable, the electro-adsorption is finished.
Preferably, the method for preparing the carbon aerogel in step (1) comprises the following steps:
mixing resorcinol, formaldehyde and acetic acid to obtain a precursor solution;
and mixing the precursor solution with water to obtain the carbon aerogel.
The invention provides a method for removing uranium element in water by electric adsorption, which comprises the following steps: (1) in CO2Thermally activating the carbon aerogel in the atmosphere to obtain activated carbon aerogel; (2) and the activated carbon aerogel is used as an electrode material, the activated carbon aerogel is assembled into an electric adsorption module, and voltage is applied to the electric adsorption module to enable uranium-containing water to circularly pass through the electric adsorption module for electric adsorption. The invention takes carbon aerogel as raw material for electric adsorption, and the carbon aerogel is treated by CO2After thermal activation, the uranium-doped carbon material has rich mesoporous structure, the specific surface area is increased, and the adsorption effect on uranium in the electric adsorption process is improved; the uranium element is removed by utilizing the electric adsorption, an electric field is formed between the electrodes in the electric adsorption process, uranium-containing water flows between the electric adsorption modules, uranium ions in the water move to the surface of the activated carbon aerogel electrode with opposite charges through the electric field force and are finally adsorbed in the pores of the activated carbon aerogel, and therefore the total concentration of the uranium element in the water is reduced. The method provided by the invention is simple to operate, has low cost and is suitable for large-scale popularization and application.
Drawings
FIG. 1 is a scanning electron micrograph of an activated carbon aerogel obtained in example 1;
FIG. 2 is a scanning electron micrograph of manganese dioxide-modified activated carbon aerogel obtained in example 1.
Detailed Description
The invention provides a method for removing uranium element in water by electric adsorption, which comprises the following steps:
(1) in CO2Thermally activating the carbon aerogel in the atmosphere to obtain activated carbon aerogel;
(2) and the activated carbon aerogel is used as an electrode material, the activated carbon aerogel is assembled into an electric adsorption module, and voltage is applied to the electric adsorption module to enable uranium-containing water to circularly pass through the electric adsorption module for electric adsorption.
The invention is in CO2And thermally activating the carbon aerogel in the atmosphere to obtain the activated carbon aerogel. In the present invention, the method for preparing the carbon aerogel preferably comprises the following steps:
mixing resorcinol, formaldehyde and acetic acid to obtain a precursor solution;
and mixing the precursor solution with water to obtain the carbon aerogel.
According to the invention, resorcinol, formaldehyde and acetic acid are preferably mixed to obtain a precursor solution. In the present invention, acetic acid is used as a catalyst. In the present invention, the molar ratio of resorcinol to formaldehyde is preferably 1: 2; the mass ratio of acetic acid to resorcinol is preferably 1: 0.75. The invention does not require any particular mixing means, such as stirring, known to the person skilled in the art.
After the precursor solution is obtained, the precursor solution is mixed with water to obtain the carbon aerogel. In the invention, the mixing temperature is preferably room temperature, the time is preferably 25-60 min, and more preferably 30min, and in the mixing process, the precursor solution undergoes a water-activating reaction to obtain the carbon aerogel.
The invention is in CO2And thermally activating the carbon aerogel in the atmosphere to obtain the activated carbon aerogel. In the invention, the temperature of thermal activation is preferably 800-1000 ℃, and more preferably 900-950 ℃; the time of the thermal activation is preferably 1.5-3 h, and more preferably 2 h. In the invention, the heating rate of heating to the thermal activation temperature is preferably 15-30 ℃/min, and the methodThe invention starts to calculate the thermal activation time after the temperature is raised to the thermal activation temperature. In the present invention, carbon aerogel is treated with CO2After thermal activation, the carbon nano-tube has rich mesoporous structure, increases the specific surface area and improves the adsorption effect in the electric adsorption process.
In the invention, the specific surface area of the activated carbon aerogel is preferably 1200-2000 cm2·g-1More preferably 1500 to 1800cm2·g-1(ii) a The total pore volume is preferably 1.5-3 cm3·g-1More preferably 2 to 2.5cm3·g-1. In the invention, the activated carbon aerogel has rich pore structures and has micropore, mesopore and macropore structures, wherein the pore diameter of the micropore is preferably 0.5-2 nm, the pore diameter of the mesopore is preferably 3-10 nm, and the pore diameter of the macropore is preferably 50-100 nm.
After the activated carbon aerogel is obtained, the activated carbon aerogel is preferably modified by the method, wherein the method for modifying comprises the following steps:
and ultrasonically mixing the activated carbon aerogel with a soluble divalent manganese salt and a potassium permanganate solution, and carrying out solid-liquid separation to obtain the manganese dioxide modified activated carbon aerogel.
In the present invention, the soluble divalent manganese salt is preferably manganese acetate. In the invention, the mass ratio of the activated carbon aerogel to the soluble divalent manganese salt is preferably 1: 0.15-0.4, and more preferably 1: 0.2. In the invention, the mass concentration of the potassium permanganate solution is preferably 15%, and the volume ratio of the mass of the activated carbon aerogel to the potassium permanganate solution is preferably 1: 25.
In the present invention, the power of the ultrasonic mixing is preferably 300W, and the time is preferably 2.5 h. In the present invention, the solid-liquid separation is preferably performed by filtration. After the filtration, the solid obtained after the filtration is preferably washed and dried by the present invention to obtain manganese dioxide modified activated carbon aerogel. In the present invention, the washing method is preferably water washing, and the drying method is not particularly limited, and the solid may be dried to a constant weight by using a drying method known to those skilled in the art.
In the invention, after the activated carbon aerogel is modified by manganese dioxide, the capacitance of an electrode material in an electric adsorption process can be improved, and the adsorption efficiency of uranium is further improved.
The method takes activated carbon aerogel as an electrode material, the activated carbon aerogel is assembled into an electro-adsorption module, voltage is applied to the electro-adsorption module, and uranium-containing water is circulated through the electro-adsorption module to carry out electro-adsorption. In the invention, the activated carbon aerogel can be directly used as an electrode material, and can also be mixed with conductive carbon black and polytetrafluoroethylene to prepare a composite electrode material. In the invention, the mass ratio of the activated carbon aerogel to the conductive carbon black and the polytetrafluoroethylene in the composite electrode material is preferably 8:1: 1.
The invention has no special requirements on the specific method for assembling the activated carbon aerogel into the electro-adsorption module, and the assembling mode known by the technicians in the field can be used.
In the present invention, the voltage applied during the electro-adsorption is preferably 0.8 to 1.4V, and more preferably 1 to 1.2V.
In the invention, the content of uranium ions in the uranium-containing water is preferably 80-140 mg/L, and more preferably 100-120 mg/L. In the invention, the speed of the uranium-containing water passing through the electric adsorption module is preferably 10-25 mL/min, and more preferably 15-20 mL/min. The invention preferably uses a peristaltic pump to effect circulation of the uranium containing water. The conductivity of the uranium-containing water is preferably monitored in the process of electric adsorption, when the conductivity of the uranium-containing water is not changed, the electrode reaches adsorption balance, and the electric adsorption is finished.
In the present invention, the activated carbon aerogel electrode can be subjected to desorption regeneration. In the present invention, the desorption regeneration method preferably includes:
and removing the voltage applied on the electro-adsorption module, desorbing, and obtaining the regenerated activated carbon aerogel electrode when the conductivity of the uranium-containing water is stable.
The method for removing uranium element from water by electro-adsorption provided by the present invention is described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Under the condition of taking acetic acid as a catalyst, resorcinol and formaldehyde are mixed in a ratio of 1:2, dissolving in deionized water at room temperature, and stirring for 30 minutes to prepare the carbon aerogel.
And (3) putting the carbon aerogel in a carbon dioxide atmosphere, and activating for 2 hours at 950 ℃ to obtain the activated carbon aerogel. The scanning electron micrograph of the obtained activated carbon aerogel is shown in FIG. 1. As can be seen from fig. 1, the specific surface area of the gel produced is large, and the capacity for adsorbing uranium is correspondingly increased.
The specific surface area of the obtained activated carbon aerogel is 1200-2000 cm through detection2·g-1The total pore volume is 1.5-3 cm3·g-1。
Preparing the activated carbon aerogel into an electrode of 1cm multiplied by 1cm, assembling the electrode into an electric adsorption module, and carrying out electric adsorption on uranium-containing water (VI-valent uranium). The voltage during electro-adsorption is 0.8V, the inflow rate is 40mL/min, and the uranium adsorption rates under different uranium concentrations are shown in Table 1. The calculation method of the uranium adsorption rate comprises the following steps: the ratio of the tail liquid uranium content after adsorption to the initial uranium content is subtracted from the initial uranium content.
TABLE 1 adsorption rate of uranium at different uranium concentrations
| Initial content (mg/L) | 140 | 120 | 100 | 80 |
| Uranium adsorption (%) | 26.52 | 38.26 | 43.66 | 35.63 |
Example 2
Activated carbon aerogel was prepared according to the method of example 1, prepared into 1cm × 1cm electrodes, assembled into an electro-adsorption module, and subjected to electro-adsorption of uranium-containing water. The concentration of uranium (VI) in the uranium-containing water is 100mg/L, the applied working voltage is 1.2V, and the uranium adsorption rates under different inflow rates are shown in Table 2.
TABLE 2 uranium adsorption Rate at different influent flow rates
| Inflow (mL/min) | 10 | 15 | 20 | 25 |
| Uranium adsorption (%) | 28.56 | 33.49 | 45.89 | 20.15 |
Example 3
Activated carbon aerogel was prepared according to the method of example 1, prepared into 1cm × 1cm electrodes, assembled into an electro-adsorption module, and subjected to electro-adsorption of uranium-containing water. The uranium (VI) concentration in the uranium-containing water is 100mg/L, the water inlet flow is controlled at 20mL/min, and the uranium adsorption rates under different applied voltages are shown in Table 3.
TABLE 3 uranium adsorption Rate at different applied voltages
| Operating voltage (V) | 0 | 0.8 | 1 | 1.2 | 1.4 |
| Uranium adsorption (%) | 6.98 | 28.26 | 35.68 | 45.35 | 38.56 |
Example 4
Activated carbon aerogel was prepared by the method of example 1, and prepared into 1cm × 1cm electrodes, which were assembled into an electrosorption module, and an operating voltage of 1.2V was applied thereto while controlling a water inflow rate of 20mL/min, thereby electrosorpting 100mg/L of uranium-containing water. After the completion of the electro-adsorption, the applied voltage is removed and desorption is performed. The electric adsorption-desorption is carried out in a circulating manner, the uranium adsorption rate and the uranium desorption rate in each circulating process are calculated, and the obtained results are shown in table 4.
TABLE 4 uranium adsorption and desorption rates at different cycle times
| Number of cycles | 1 | 2 | 3 | 4 | 5 | 6 |
| Uranium adsorption (%) | 47.49 | 45.33 | 45.63 | 43.42 | 43.32 | 42.89 |
| Uranium desorption rate (%) | 76.88 | 76.23 | 76.21 | 76.21 | 76.93 | 76.69 |
As can be seen from table 4, after the first cycle experiment, the adsorption rate of uranium is 47.49%, and after 6 cycles of experiment, the removal rate is only reduced by 9.6%, indicating that the activated carbon aerogel electrode has excellent regeneration capability.
Example 5
Activated carbon aerogel was prepared in the same manner as in example 1, and 5g of the activated carbon aerogel was mixed with Mn (Ac)2·4H2Mixing O at a mass ratio of 1:0.2, adding 125mL of 15% KMnO4And (3) sequentially carrying out ultrasonic treatment, standing, washing, drying and grinding on the solution to obtain the manganese dioxide modified activated carbon aerogel. The scanning electron microscope image of the manganese dioxide modified activated carbon aerogel is shown in fig. 2, and as can be seen from fig. 2, the specific surface area of the activated carbon aerogel is larger, so that the uranium adsorption capacity of the material is greatly improved.
Mixing the obtained manganese dioxide modified activated carbon aerogel with conductive carbon black and polytetrafluoroethylene according to the mass ratio of 8:1:1, fully mixing to prepare a composite electrode material, and casting the composite electrode material on a graphite film current collector to prepare a carbon aerogel/manganese dioxide composite electrode.
Assembling the carbon aerogel/manganese dioxide composite material electrode into an electric adsorption module, and carrying out electric adsorption on uranium-containing water (VI-valent uranium). The voltage during electro-adsorption is 0.8V, the inflow rate is 40mL/min, and the uranium adsorption rates under different uranium concentrations are shown in Table 5.
TABLE 5 uranium adsorption Rate at different uranium concentrations
| Initial content (mL/min) | 140 | 120 | 100 | 80 |
| Uranium adsorption (%) | 28.32 | 40.21 | 47.68 | 37.56 |
Example 6
A carbon aerogel/manganese dioxide composite electrode was prepared as in example 5. Assembling the carbon aerogel/manganese dioxide composite material electrode into an electric adsorption module, and carrying out electric adsorption on uranium-containing water. The concentration of uranium (VI) in the uranium-containing water is 100mg/L, the applied working voltage is 1.2V, and the uranium adsorption rates under different inflow rates are shown in Table 6.
TABLE 6 uranium adsorption Rate at different influent flow rates
| Inflow rate of water | 10 | 15 | 20 | 25 |
| Uranium adsorption (%) | 30.54 | 37.43 | 47.89 | 22.45 |
Example 7
A carbon aerogel/manganese dioxide composite electrode was prepared as in example 5. Assembling the carbon aerogel/manganese dioxide composite material electrode into an electric adsorption module, and carrying out electric adsorption on uranium-containing water. The uranium (VI) concentration in the uranium-containing water is 100mg/L, the water inlet flow is controlled at 20mL/min, and the uranium adsorption rates under different applied voltages are shown in Table 7.
TABLE 7 uranium adsorption Rate at different applied voltages
| Operating voltage (V) | 0 | 0.8 | 1 | 1.2 | 1.4 |
| Uranium adsorption (%) | 8.96 | 31.24 | 36.78 | 48.38 | 39.54 |
Example 8
Activated carbon aerogel was prepared by the method of example 1, and prepared into 1cm × 1cm electrodes, which were assembled into an electrosorption module, and an operating voltage of 1.2V was applied thereto while controlling a water inflow rate of 20mL/min, thereby electrosorpting 100mg/L of uranium-containing water. After the completion of the electro-adsorption, the applied voltage is removed and desorption is performed. The electric adsorption-desorption was performed cyclically, and the uranium adsorption rate and uranium desorption rate in each cycle were calculated, and the obtained results are shown in table 8.
TABLE 8 uranium adsorption and desorption rates at different cycle times
| Number of cycles | 1 | 2 | 3 | 4 | 5 | 6 |
| Uranium adsorption (%) | 49.43 | 48.32 | 47.65 | 46.44 | 45.51 | 44.88 |
| Uranium desorption rate (%) | 78.66 | 79.32 | 79.22 | 80.01 | 79.33 | 79.96 |
As can be seen from table 8, after one cycle experiment, the adsorption rate was 49.43%, and after 6 cycles of experiment, the removal rate was only reduced by 4.55%, indicating that the manganese dioxide modified activated carbon aerogel electrode has excellent regeneration capability.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for removing uranium element in water by electro-adsorption comprises the following steps:
(1) in CO2Thermally activating the carbon aerogel in the atmosphere to obtain activated carbon aerogel;
(2) and assembling the activated carbon aerogel into an electric adsorption module by taking the activated carbon aerogel as an electrode, and applying voltage on the electric adsorption module to enable the uranium-containing water to circularly pass through the electric adsorption module for electric adsorption.
2. The method according to claim 1, wherein the temperature of the thermal activation in the step (1) is 800-1000 ℃ and the time is 1.5-3 h.
3. The method of claim 1 or 2, wherein the activated carbon aerogel has a specific surface area of 1200 to 2000cm2·g-1The total pore volume is 1.5-3 cm3·g-1。
4. The method of claim 1, further comprising, prior to said assembling, modifying said activated carbon aerogel, said modifying comprising:
and ultrasonically mixing the activated carbon aerogel with a soluble divalent manganese salt and a potassium permanganate solution, and carrying out solid-liquid separation to obtain the manganese dioxide modified activated carbon aerogel.
5. The method of claim 4, wherein the mass ratio of the activated carbon aerogel to the soluble divalent manganese salt is 1: 0.15-0.4.
6. The method according to claim 1 or 4, wherein the applied voltage is 0.8 to 1.4V.
7. The method according to claim 1, wherein the content of uranium ions in the uranium-containing water is 10-200 mg/L.
8. The method according to claim 1 or 7, wherein the rate of uranium containing water passing through the electro-adsorption module is 10-25 mL/min.
9. The method of claim 1, wherein the electro-adsorption process further comprises monitoring the conductivity of the uranium-containing water during electro-adsorption, and the electro-adsorption is terminated when the conductivity of the uranium-containing water is stable.
10. The method according to claim 1 or 4, wherein the method for preparing the carbon aerogel in the step (1) comprises the following steps:
mixing resorcinol, formaldehyde and acetic acid to obtain a precursor solution;
and mixing the precursor solution with water to obtain the carbon aerogel.
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Citations (4)
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|---|---|---|---|---|
| JPH09202610A (en) * | 1996-01-24 | 1997-08-05 | Mitsubishi Chem Corp | Activated carbon and its production |
| CN104098086A (en) * | 2014-07-18 | 2014-10-15 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of carbon aerogel with high absorption property |
| CN108285195A (en) * | 2018-01-10 | 2018-07-17 | 大连理工大学 | The preparation and application of the electrode material of carbon aerogel load manganese dioxide |
| CN111875006A (en) * | 2020-07-10 | 2020-11-03 | 东华理工大学 | Preparation method of biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode |
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- 2021-08-05 CN CN202110894539.6A patent/CN113582300B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09202610A (en) * | 1996-01-24 | 1997-08-05 | Mitsubishi Chem Corp | Activated carbon and its production |
| CN104098086A (en) * | 2014-07-18 | 2014-10-15 | 天津得瑞丰凯新材料科技有限公司 | Preparation method of carbon aerogel with high absorption property |
| CN108285195A (en) * | 2018-01-10 | 2018-07-17 | 大连理工大学 | The preparation and application of the electrode material of carbon aerogel load manganese dioxide |
| CN111875006A (en) * | 2020-07-10 | 2020-11-03 | 东华理工大学 | Preparation method of biomass source N, P co-doped carbon aerogel/cross-linked chitosan composite membrane electrode |
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