CN112354528A - Phosphoric acid functionalized sponge composite material for extracting uranium from seawater and preparation method thereof - Google Patents
Phosphoric acid functionalized sponge composite material for extracting uranium from seawater and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which comprises the following steps: weighing sodium phytate, adding the sodium phytate into water, and stirring until the sodium phytate is completely dissolved to obtain a sodium phytate aqueous solution; putting melamine sponge into a prepared sodium phytate aqueous solution, completely soaking, carrying out hydrothermal reaction at a certain temperature and pressure for a period of time, and cooling to room temperature; and taking out the phosphoric acid functionalized melamine sponge, washing the melamine sponge with deionized water to be neutral, and drying in vacuum to obtain the phosphoric acid functionalized sponge composite material. The method uses commercial melamine sponge as a material framework, uses a sodium phytate aqueous solution as a functional adsorbent, and self-assembles a macroscopic three-dimensional network sponge porous adsorption material through hydrothermal reaction, has the advantages of simple process, wide raw material source, low cost, no toxicity and harm, and easy large-scale popularization, and the prepared phosphoric acid functionalized sponge composite material has good mechanical property, large specific surface area and loose porous structure, and the maximum saturated adsorption capacity of uranium reaches 537.98 mg/g.
Description
Technical Field
The invention relates to the field of novel materials, in particular to a phosphoric acid functionalized sponge composite material for extracting uranium from seawater and a preparation method thereof.
Background
Uranium is a strategic resource on which the nuclear industry is dependent to develop, and compared with the ambitious nuclear energy development and planning, the uranium fuel in China has serious self-sufficiency and is unfavorable for guaranteeing the energy safety. Meanwhile, uranium has double hazards of heavy metal chemical toxicity and radioactivity, and the World Health Organization (WHO) determines that the maximum pollution upper limit of uranium in domestic water is 30 mu g/L, while the concentration of uranium in uranium-containing water bodies produced in the uranium ore industry and the nuclear industry far exceeds the limit. Therefore, the efficient enrichment and extraction of uranium resources from uranium-containing water bodies (such as natural seawater, uranium mining and metallurgy and nuclear industrial wastewater) has important significance for the sustainable development of energy and environment. Two key strategies for improving adsorption performance of uranium adsorbents are generally (1) altering the surface chemical groups of the adsorbent to increase uranyl ion affinity: usually, the modification is realized by amidoxime or phosphate radical; (2) increase of adsorbent surface area: the specific surface area is increased by introducing as much pore structure as possible or reducing the size of the adsorbent, thereby maximizing the adsorption sites per mass of the adsorbent.
In the current research progress, there are many novel porous functional materials such as porous organic polymer materials (POPs), metal organic framework Materials (MOFs), covalent organic framework materials (COFs), Graphene Oxide (GO) -based materials, layered metal sulfides, mesoporous silica, porous carbon materials, etc. applied in the uranium adsorption field, although the high specific surface area characteristics of these materials have obvious advantages for improving the uranium adsorption capacity, the above materials generally exist in the state of micro-nano particles or powder, and there are obvious limitations in the actual use and recovery process.
In recent years, fiber materials are also gradually and widely used for removing uranyl ions in uranium extraction from seawater and other uranium-containing water bodies, the fiber materials well solve the problems of operation and recovery in the use process, however, high-performance fiber adsorbing materials are complex in preparation process, and the problems that the adsorption efficiency and the mechanical property are difficult to take into account exist simultaneously.
The sponge elastic material is a good uranium adsorbing material system, the specific surface area of a porous framework of the sponge elastic material is large, and if in earlier researches, a novel uranium adsorbing material (CN201810383228.1) with mechanical flexibility and high adsorption capacity is obtained by coating an amidoxime-containing polyacrylonitrile hydrogel coating on the surface of a three-dimensional framework of the porous structure elastic material. In addition, related reports in the same lines also disclose a preparation and uranium adsorption method (CN201810342054.4) of L-arginine modified graphene oxide sponge, a modified polyacrylonitrile porous foamed uranium adsorption material containing amidoxime groups and a preparation method (CN201910269877.3), and although the material has good uranium adsorption effect, improvements are still needed in the aspects of adsorption efficiency, manufacturing cost, macro-quantization manufacturing capability and the like.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which solves the problems of low adsorption efficiency or poor mechanical strength of the existing uranium extracting material.
On one hand, the invention adopts a preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which comprises the following steps:
s101, weighing sodium phytate, adding the sodium phytate into water, and stirring until the sodium phytate is completely dissolved to obtain a sodium phytate aqueous solution;
s102, putting melamine sponge into a prepared sodium phytate aqueous solution, completely soaking, carrying out hydrothermal reaction at a certain temperature and pressure for a period of time, and cooling to room temperature;
s103, taking out the phosphoric acid functionalized melamine sponge, washing the melamine sponge with deionized water to be neutral, and drying in vacuum to obtain the phosphoric acid functionalized sponge composite material.
Preferably, in the step S101, the pH of the sodium phytate aqueous solution is 4.
Preferably, in the step S101, the mass concentration of the sodium phytate aqueous solution is 5%.
Preferably, in the S102 step, the hydrothermal reaction temperature is 95 ℃ and the pressure is 1.0 MPa.
Preferably, in the step S102, the hydrothermal reaction time is 12 h.
Preferably, in the step S102, the density of the melamine sponge is 0.74 × 10-2g/cm3。
Preferably, in the step S103, the vacuum drying temperature is 70 ℃ and the time is 8 h.
On the other hand, the phosphate functionalized sponge composite material for extracting uranium from seawater is also provided.
According to the preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which is provided by the invention, commercial melamine sponge is used as a material framework, a sodium phytate aqueous solution is used as a functional adsorbent, and a uranium adsorbing material with a phosphoric acid functionalized sponge structure is prepared by a hydrothermal method; the method is characterized in that nitrogen and hydrogen in the melamine sponge, oxygen and hydrogen atoms and phosphate radicals in sodium phytate molecules are respectively induced to be subjected to non-covalent bonding self-assembly in the hydrothermal reaction process, a supermolecule coating layer structure is generated on the surface of a melamine sponge framework, and finally the macroscopic three-dimensional network-shaped sponge porous adsorption material is obtained.
Furthermore, the phosphoric acid functionalized sponge composite material prepared by the invention has good mechanical property, large specific surface area and loose porous structure, is beneficial to adsorption of uranyl ions, and can reach a saturated adsorption quantity of more than 500mg/g within a few minutes.
Drawings
FIG. 1 is an infrared absorption spectrum diagram of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, wherein a represents melamine sponge; b represents a phosphoric acid functionalized sponge composite material;
FIG. 2 is a scanning electron microscope image of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, wherein a and b represent melamine sponge; c and d represent phosphoric acid functionalized sponge composite materials;
FIG. 3 is a graph of a representative uranium adsorption kinetics test result of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, wherein in 8ppm simulated seawater (1L) doped with uranium, equilibrium is achieved within 10min of adsorption, and at the moment, the equilibrium adsorption amount is 290.76 mg/g;
FIG. 4 is a graph showing the result of a representative saturated adsorption capacity test of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater, and the maximum saturated adsorption capacity of uranium is 537.98mg/g when an isothermal adsorption test is carried out in simulated uranium-doped seawater (1L) with different uranium concentrations (4-64 ppm).
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The raw materials of the sodium phytate, the melamine sponge (melamine-formaldehyde resin) and the like are all commercial products.
The first embodiment is as follows: a preparation method of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater comprises the following steps:
s101 preparation of a phosphoric acid group-containing aqueous solution: weighing 2g of sodium Phytate (PAS) according to the weight part ratio, adding the PAS into 38g of deionized water, and magnetically stirring for 5min at room temperature until the PAS is completely dissolved, wherein the pH value of the sodium phytate solution in the step is measured to be 4;
s102 phosphoric acid functionalization reaction: then, 2.5 × 1.5cm of melamine sponge (mass 69.1mg, density 0.74 × 10)-2g/cm3) Putting the mixture into a phosphate group aqueous solution for complete soaking, carrying out hydrothermal reaction for 12 hours in a closed reaction container with the temperature of 95 ℃ and the pressure of 1.0MPa, and cooling to room temperature after the reaction is finished;
s103, washing, drying and post-treatment: and taking out the phosphoric acid functionalized melamine sponge, washing the melamine sponge with deionized water for multiple times until the melamine sponge is neutral, and drying the melamine sponge in vacuum for 8 hours at the temperature of 70 ℃ to obtain the phosphoric acid functionalized sponge composite material.
(1) The phosphoric acid functionalized sponge composite material of the first embodiment is characterized by infrared spectroscopy and scanning electron microscopy, and as shown in the infrared spectroscopy result of figure 1, compared with the infrared spectroscopy peak of melamine sponge, the phosphoric acid functionalized sponge composite material is obviously seen to have P-O-H (1625 cm)-1)、P-O-C(1060cm-1) And P ═ H (1152 cm)-1) Infrared absorption peak proves that the melamine sponge porous composite material with phosphate radical is successfully prepared, as shown in a scanning electron microscope picture of figure 2, compared with a melamine sponge structure, the phosphate functionalized sponge composite material keeps a uniform three-dimensional macroporous structure, and a supermolecular film structure formed by self-assembly of phytic acid molecules can be obviously seen on the surface of a sponge framework.
(2) The phosphorus acid functionalized sponge composite material of the first embodiment is subjected to uranium adsorption performance test: firstly, 15mg of the phosphoric acid functionalized sponge composite material is placed in simulated seawater (1L) doped with uranium (8ppm) for adsorption kinetics examination, and the equilibrium is found within 10min of adsorption, as shown in figure 3, the equilibrium adsorption amount is 290.76 mg/g; and then placing 15mg of the phosphoric acid functionalized sponge composite material in 1L of uranium-doped simulated seawater with different uranium concentrations (4-64ppm) for saturated adsorption capacity examination, wherein the result is shown in figure 4, and the maximum saturated adsorption capacity is 537.98 mg/g.
Example two: the difference between the second embodiment and the first embodiment is that the sodium phytate used in the step S101 is 0%, 0.5%, 1.0%, 2.5%, 7.5% and 10.0% by mass in the aqueous solution, respectively. The optimal concentration of the sodium phytate raw material is 5.0%.
TABLE 1 Effect of different sodium phytate concentrations on the Performance of phosphoric acid functionalized sponge composites
As can be seen from table 1, with the increase of the sodium phytate concentration, the adsorption capacity of the prepared material uranyl ions gradually increases and reaches the maximum at 5.0%, when the sodium phytate concentration in the raw material reaches 10.0%, the melamine sponge is found to melt and disappear in the reaction solution after the reaction is completed, and at the 7.5% sodium phytate concentration, the adsorption capacity of the product uranium is obviously reduced when being compared with 5.0%, and it is possible that when the sodium phytate concentration is too high, phosphate ions and water molecules can form self-assembled supermolecules through hydrogen bond bonding, so that the uranium adsorption active sites of the product are reduced, and when the sodium phytate concentration is 7.5%, the three-dimensional framework strength of the melamine sponge is obviously destroyed, so that the mechanical properties of the product are reduced.
Example three: the difference between the third embodiment and the first embodiment is that the hydrothermal reaction temperature in step S102 is 25 ℃, 60 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃ and 110 ℃.
TABLE 2 Effect of different hydrothermal reaction temperatures on the Properties of phosphoric acid functionalized sponge composites
| Reaction temperature (. degree.C.) | Uranium adsorption capacity (mg-U/g-sponge) |
| 25 | 5.0 |
| 60 | 100.05 |
| 75 | 216.67 |
| 80 | 191.46 |
| 85 | 244.26 |
| 90 | 343.64 |
| 95 | 537.98 |
| 100 | 204.32 |
| 105 | 100.52 |
| 110 | -- |
It can be seen from table 2 that the increase of the hydrothermal reaction temperature is beneficial to the improvement of the adsorption performance of the product uranium, sodium phytate and melamine sponge can not react at room temperature (25 ℃), and when the reaction temperature is 95 ℃, the adsorption capacity of uranium in the prepared phosphoric acid functionalized sponge composite material is maximum, but when the reaction temperature is too high (more than 105 ℃, namely 110 ℃), the melamine sponge can be dissolved in the reaction solution, and is not suitable for modification reaction.
Example four: the difference between the fourth example and the first example is that the hydrothermal reaction time in step S102 is 0h, 3h, 6h, 9h, 10h, 11h, 12h, 13h, 14h and 15h, respectively. The optimal reaction time is 12 h.
TABLE 3 Effect of different hydrothermal reaction times on the Properties of phosphoric acid functionalized sponge composites
| Reaction time (h) | Uranium adsorption capacity (mg-U/g-sponge) |
| 0 | 5.0 |
| 3 | 94.32 |
| 6 | 134.52 |
| 9 | 229.05 |
| 10 | 346.67 |
| 11 | 414.26 |
| 12 | 537.98 |
| 13 | 523.64 |
| 14 | 542.64 |
| 15 | 533.32 |
It can be seen from table 3 that the extension of modified reaction time is favorable to the promotion of product uranium adsorption performance, and when 12h, the phosphoric acid functional sponge composite uranium adsorption capacity of preparing reaches the biggest, but continues extension reaction time (being greater than 12h), and phosphoric acid functional sponge composite uranium adsorption capacity tends to the mild, from this can know, reaches best reaction time when about 12 h.
Example five: the difference between the fifth example and the first example is that in the step S101, the pH of the aqueous solution containing phosphate groups is varied by adding sodium hydroxide dropwise to the phytic acid solution while the phosphate group concentration is unchanged, and adjusting the pH.
TABLE 4 Effect of pH of aqueous solutions containing phosphate groups on the Performance of phosphate-functionalized sponge composites
As can be seen from table 4, when the pH is 1, the melamine sponge is corroded and decomposed in the reaction process due to too strong acidity, and the uranium adsorption performance of the phosphate-functionalized sponge composite material is gradually improved with the increase of the pH of the phosphate-based aqueous solution, and when the pH is about 4, the uranium adsorption capacity of the prepared phosphate-functionalized sponge composite material reaches the maximum, but the uranium adsorption capacity of the obtained phosphate-functionalized sponge composite material is gradually reduced with the continuous increase of the pH of the phosphate-based aqueous solution, which indicates that the uranium extraction effect of the phosphate-functionalized sponge composite material prepared when the pH is 4 is the best.
In conclusion, according to the preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which is provided by the invention, commercial melamine sponge is used as a material framework, a sodium phytate aqueous solution is used as a functional adsorbent, and a uranium adsorbing material with a phosphoric acid functionalized sponge structure is prepared by a hydrothermal method; the method is characterized in that nitrogen and hydrogen in the melamine sponge, oxygen and hydrogen atoms and phosphate radicals in sodium phytate molecules are respectively induced to be subjected to non-covalent bonding self-assembly in the hydrothermal reaction process, a supermolecule coating layer structure is generated on the surface of a melamine sponge framework, and finally the macroscopic three-dimensional network-shaped sponge porous adsorption material is obtained.
Furthermore, the phosphoric acid functionalized sponge composite material prepared by the invention has good mechanical property, large specific surface area and loose porous structure, is beneficial to adsorption of uranyl ions, and can reach a saturated adsorption quantity of more than 500mg/g within a few minutes.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A preparation method of a phosphoric acid functionalized sponge composite material for extracting uranium from seawater is characterized by comprising the following steps:
s101, weighing sodium phytate, adding the sodium phytate into water, and stirring until the sodium phytate is completely dissolved to obtain a sodium phytate aqueous solution;
s102, putting melamine sponge into the sodium phytate aqueous solution prepared in the step S101, completely soaking, carrying out hydrothermal reaction at a certain temperature and pressure for a period of time, and cooling to room temperature;
s103, taking out the phosphoric acid functionalized melamine sponge, washing the melamine sponge with deionized water to be neutral, and drying in vacuum to obtain the phosphoric acid functionalized sponge composite material.
2. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S101, the pH of the sodium phytate aqueous solution is 4.
3. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S101, the mass concentration of the sodium phytate aqueous solution is 5%.
4. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S102, the hydrothermal reaction temperature is 95 ℃ and the pressure is 1.0 MPa.
5. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S102, the hydrothermal reaction time is 12 h.
6. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S102, the density of the melamine sponge is 0.74 x 10-2g/cm3。
7. The preparation method of the phosphoric acid functionalized sponge composite material for extracting uranium from seawater according to claim 1, which is characterized by comprising the following steps: in the step S103, the vacuum drying temperature is 70 ℃ and the time is 8 h.
8. A phosphoric acid functionalized sponge composite material for extracting uranium from seawater, which is prepared according to the method of any one of claims 1 to 7.
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| CN113000034A (en) * | 2021-02-23 | 2021-06-22 | 浙江理工大学 | Preparation method of uranium ion affinity membrane based on natural plant polyphenol composite coating |
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