CN115477374A - MoO (MoO) 2 Preparation and application methods of @ NHCS hollow structure material - Google Patents
MoO (MoO) 2 Preparation and application methods of @ NHCS hollow structure material Download PDFInfo
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- CN115477374A CN115477374A CN202210858573.2A CN202210858573A CN115477374A CN 115477374 A CN115477374 A CN 115477374A CN 202210858573 A CN202210858573 A CN 202210858573A CN 115477374 A CN115477374 A CN 115477374A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4691—Capacitive deionisation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a MoO 2 The preparation method of the @ NHCS nano material comprises the steps of strongly stirring a mixed solution containing tetraethyl silicate, ethanol, ammonia water and deionized water, adding a dopamine hydrochloride solution into the mixed solution, stirring, centrifuging the mixed solution after reaction is finished, and collecting a product SiO 2 @ PDA and washed, then dried; the prepared SiO is mixed 2 Calcining @ PDA in nitrogen atmosphere to form nitrogen-doped silicon dioxide carbon spheres; dispersing the obtained product into hydrofluoric acid aqueous solution, continuously stirring, centrifugally collecting, and drying to obtain nitrogen-doped hollow carbon spheres; dispersing ammonium molybdate into a mixed solvent of deionized water and ethylene glycol, adding the prepared nitrogen-doped hollow carbon spheres, performing ultrasonic treatment, pouring the mixture into a high-pressure reaction kettle for reaction, collecting and washing the obtained solid with the deionized water and ethanol, and calcining the solid in a nitrogen atmosphere to obtain the molybdenum dioxide coupled nitrogen-doped hollow carbon spheres. The nano material of the inventionMaterial for removing Pb in water body by using capacitive deionization method 2+ In this case, high removal efficiency can be achieved.
Description
Technical Field
The invention relates to a preparation method and an application method of a nano material, in particular to a MoO 2 Preparation of @ NHCS hollow structure material and preparation method thereofAn application method.
Background
Along with the rapid growth of population and the continuous expansion of cities, the problems of excessive energy consumption and environmental pollution follow, so that the contradiction between supply and demand of drinking water in the world is more prominent. Water pollution and shortage of clean water will be a great challenge to the world. Heavy metals are ubiquitous in water and are the most common nuisance harming human health and ecological environment. Lead is a main toxic metal pollutant in underground water, is recognized as a chemical pollutant causing public health problems by world health organization, is difficult to degrade, can cause serious damage to human bodies in trace amount, and directly influences organisms, kidneys, livers, reproductive systems, nervous systems and the like. Therefore, it is of great significance to develop an environment-friendly and efficient lead ion water treatment method.
In recent years, various effective methods for removing lead ions from water have been proposed, such as adsorption, chemical precipitation, ion exchange, phytoremediation, and membrane separation. In addition, various materials have been explored as adsorbents for capturing lead ions in aqueous environments, such as metal oxide nanostructures and metal hydroxides. However, these methods require extensive pretreatment steps and chemical additives, and the adsorbent is also unstable in solution, making it difficult to completely remove lead ions from the solution. Meanwhile, various heavy metal ions are also present in the wastewater, so that it is difficult to selectively remove lead ions in the wastewater. Therefore, it is necessary to develop an effective selective lead removal technology to achieve sustainable development of the environment.
Capacitive Deionization (CDI) technology originated in the last 70 th century and its working principle is shown in fig. 1: mainly through applying voltage on two ends of the electrode, double electric layers are formed on the surface of the electrode material and in the pore channels, so that charged ions are removed from the solution, the ions are temporarily fixed in the solution, and the regeneration and energy recovery of the electrode are achieved through short circuit or reverse voltage application. According to the above working principle, in the CDI device, the electrode is a key part for realizing the whole ion adsorption and desorption process. Compared with other methods, the method has the advantages of low energy consumption, easy regeneration, environmental protection and the like due to the unique working principle. At present, the capacitive deionization technology is mostly used in the field of desalination, and reports on the aspect of removing heavy metals are few, so that the method for selectively removing heavy metal ions by adopting the capacitive deionization technology is a novel and attractive method.
Disclosure of Invention
The invention aims to provide a MoO 2 Preparation and application methods of the @ NHCS hollow structure material. The method develops an anode material with low price, simple preparation method and high efficiency, and the anode material is used for removing Pb in water by a capacitive deionization method 2+ The method has high-efficiency removal performance, and provides an idea for removing heavy metal ions in the environmental water body.
The technical scheme of the invention is as follows: moO 2 The preparation method of the @ NHCS hollow structure material comprises the following steps:
a: firstly, intensively stirring a mixed solution containing tetraethyl silicate, ethanol, ammonia water and deionized water, then adding a dopamine hydrochloride solution into the mixed solution, stirring, centrifuging the mixed solution after the reaction is finished, and collecting a product SiO 2 @ PDA and washed, then dried;
b: prepared SiO 2 Calcining the @ PDA in nitrogen atmosphere to form nitrogen-doped silicon dioxide carbon spheres, dispersing the obtained product into hydrofluoric acid aqueous solution, continuously stirring, centrifugally collecting, and drying to obtain nitrogen-doped hollow carbon spheres;
c: dispersing ammonium molybdate into a mixed solvent of deionized water and ethylene glycol, adding the prepared nitrogen-doped hollow carbon spheres, performing ultrasonic treatment, pouring the mixture into a polytetrafluoroethylene lined high-pressure reaction kettle for reaction, collecting and washing the obtained solid with deionized water and ethanol, and calcining the solid in nitrogen atmosphere to obtain the molybdenum dioxide coupled nitrogen-doped hollow carbon spheres.
Foregoing MoO 2 In the preparation method of the @ NHCS hollow structure material, the specific preparation method comprises the following steps:
a: first, a solution containing 1mL of tetraethyl silicate, 24mL of ethanol, and 1mL of 28% NH was prepared 3 ·H 2 A mixed solution of O and 80mL of deionized water was vigorously stirred for 30min, and then 8mL and 50 mg. Multidot.mL were added -1 Dopamine hydrochloride solutionAdding the solution into the mixed solution, stirring for 24h, centrifuging the mixed solution after the reaction is finished, collecting the product, washing with deionized water and ethanol for several times, and collecting the obtained SiO 2 @ PDA, then dried at 80 ℃ for 24h;
b: prepared SiO 2 @ PDA at 800 ℃ at a temperature rise rate of 5 ℃/min, N 2 Calcining for 2 hours in the atmosphere to form nitrogen-doped silicon dioxide carbon spheres, dispersing the obtained product into 10wt% hydrofluoric acid aqueous solution, continuously stirring for 1 hour to completely remove silicon dioxide nuclei, centrifugally collecting, and drying at 80 ℃ to obtain nitrogen-doped hollow carbon spheres;
c: dispersing 0.3g of ammonium molybdate powder into a mixed solvent of 60mL of deionized water and 6mL of ethylene glycol, adding 0.06g of prepared nitrogen-doped hollow carbon spheres, carrying out ultrasonic treatment for 30min, pouring into a polytetrafluoroethylene lined high-pressure reaction kettle, heating for 10h at 150 ℃, collecting and washing the obtained solid with deionized water and ethanol, and then heating at 800 ℃ at a heating rate of 5 ℃/min and N 2 Calcining for 5 hours in the atmosphere to obtain the final product molybdenum dioxide coupled nitrogen doped hollow carbon spheres.
MoO (MoO) 2 Application method of @ NHCS hollow structure material, moO 2 The @ NHCS hollow structure material is used as an anode and applied to removal of lead ions by a capacitive deionization method.
Foregoing MoO 2 In the application method of the @ NHCS hollow structure material, the method for removing lead ions by a capacitive deionization method comprises the following steps: adding MoO 2 Mixing and stirring the @ NHCS material, the conductive carbon black, the polyvinylidene fluoride and the N-methyl pyrrolidone uniformly, and MoO 2 The mass ratio of the @ NHCS material to the conductive carbon black to the polyvinylidene fluoride is 8:1:1, then coated on graphite paper as a working electrode, and charged with Pb (NO) containing solution in a beaker 3 ) 2 The blue battery testing system applies working voltage, the peristaltic pump applies liquid circulation to carry out the capacitance deionization method to remove the Pb in the water body 2+ 。
MoO as described above 2 In the application method of the @ NHCS hollow structure material, the Pb in the water body is removed by a capacitive deionization method 2+ In the process of (1), pb 2+ The concentration is 10-100 ppm; the pH value is 3-8; the applied voltage is 0.6-1.2V.
MoO as described above 2 In the application method of the @ NHCS hollow structure material, the Pb in the water body is removed by a capacitive deionization method 2+ In the process of (1), pb 2+ The concentration is 10-100 ppm; the pH value is 6; the applied voltage was 1.2V.
The invention has the beneficial effects that: compared with the prior art, the MoO of the invention 2 The material with the @ NHCS hollow structure has the advantages that the surface area of the material is increased due to the hollow spherical structure of the material, carbon is doped, the electrochemical performance is enhanced, and the material is favorable for adapting to volume change during charge and discharge. The material prepared by the method is used for removing Pb in water body by a capacitive deionization method 2+ When the removal rate is high (10 ppm Pb), a high removal rate can be achieved 2+ The solution removal rate reaches more than 85 percent), and the energy consumption and the cost are greatly reduced.
Drawings
FIG. 1 is a MoO of the present invention 2 A synthetic schematic diagram of the @ NHCS hollow structure material;
FIG. 2 shows MoO prepared by the method of the present invention 2 The morphology characterization result of @ NHCS is shown schematically;
(in the figure, (a-b) is MoO 2 SEM of @ NHCS; (c-e) is MoO 2 TEM of @ NHCS; and (f) is MoO 2 @ NHCS element mapping of C, N, O and Mo
FIG. 3 is a diagram of the MoO prepared by the method of the present invention 2 The structural characterization result of @ NHCS is shown schematically;
(in the figure, (a) is MoO 2 XRD spectrum of @ NHCS, (b) Raman spectrum, (C) C1 s fine spectrum, (d) N1 s fine spectrum, (e) O1 s fine spectrum, (f) Mo 3d fine spectrum)
FIG. 4 shows Pb when a prepared according to the present invention is used as an anode material 2+ The removal efficiency of (2);
(in the figure, pb is present under the conditions that (a) is pH 3-8 and (b) is applied voltage of 0.6-1.2V 2+ The adsorption capacity of (a); in the figure, (c) different concentrations of Pb 2+ Adsorption capacity at concentration (pH 6 and applied voltage of 1.2V); (d) Is 10ppm of Pb 2+ (removal of pH 6 and applied voltage of 1.2V) the experiment was repeated).
Detailed Description
The invention is further illustrated by the following figures and examples, which are not to be construed as limiting the invention.
Example 1 of the invention: moO (MoO) 2 The preparation method of the @ NHCS hollow structure material is shown in figure 1, and the specific preparation method comprises the following steps:
a: first, a solution containing 1mL of tetraethyl silicate (TEOS), 24mL of ethanol, 1mL of 28% NH 3 ·H 2 A mixed solution of O and 80mL of deionized water was vigorously stirred for 30min. Then, 8mL of dopamine hydrochloride solution (50 mg. ML) was added -1 ) The mixed solution is added and stirred for 24 hours. After the reaction was completed, the mixed solution was centrifuged to collect the product, which was washed several times with deionized water and ethanol. Collecting the obtained SiO 2 @ PDA, then dried at 80 ℃ for 24h;
b: prepared SiO 2 @ PDA at 800 ℃ at a temperature rise rate of 5 ℃/min, N 2 And calcining for 2h in the atmosphere to form the nitrogen-doped silicon dioxide carbon spheres. Dispersing the obtained product into 10wt% hydrofluoric acid aqueous solution, continuously stirring for 1h, completely removing silicon dioxide nuclei, centrifugally collecting, and drying at 80 ℃ to obtain nitrogen-doped hollow carbon spheres;
c: dispersing ammonium molybdate powder (0.3 g) into a mixed solvent of 60mL deionized water and 6mL ethylene glycol, adding the prepared nitrogen-doped hollow carbon spheres (0.06 g), carrying out ultrasonic treatment for 30min, pouring into a 100mL polytetrafluoroethylene lining type high-pressure reaction kettle, and heating at 150 ℃ for 10h. Collecting and washing the resulting solid with deionized water and ethanol, then heating at 800 deg.C at a rate of 5 deg.C/min, N 2 Calcining for 5h in the atmosphere. The final product MoO is obtained 2 @NHCS。
MoO (MoO) 2 Application method of @ NHCS hollow structure material, moO 2 The @ NHCS hollow structure is used as an anode material and applied to the removal of Pb by a capacitive deionization method 2+ In (1).
The method for removing lead ions by the capacitive deionization method comprises the following steps: adding MoO 2 Mixing and stirring the @ NHCS material, the conductive carbon black, the polyvinylidene fluoride and the N-methyl pyrrolidone uniformly, and MoO 2 The mass ratio of the @ NHCS material to the conductive carbon black to the polyvinylidene fluoride is 8:1:1; then coating on stoneThe ink paper is used as a working electrode, and Pb (NO) is filled in the beaker 3 ) 2 The blue battery testing system applies working voltage, the peristaltic pump applies liquid circulation to carry out the capacitance deionization method to remove the Pb in the water body 2+ 。
Method for removing Pb in water body by capacitive deionization 2+ In the process of (1), pb 2+ The concentration is 10-100 ppm; the pH value is 3-8; the applied voltage is 0.6-1.2V.
FIG. 2 is MoO 2 Scanning Electron Micrographs (SEM) and Transmission Electron Micrographs (TEM) of @ NHCS from which MoO can be observed 2 The @ NHCS is in the shape of a hollow sphere overall, has a large specific surface area and can provide more adsorption sites. As can be seen from the element mapping graph, the prepared catalyst C, N, O and Mo have very uniform distribution.
The crystal structure of the catalyst was characterized by XRD diffraction (fig. 3 (a)), with a distinct diffraction peak for molybdenum dioxide. Further, moO 2 The XPS fine spectrum of C1 s for @ NHCS shows four main peaks at 284.8, 286, 287 and 288.7 eV (FIG. 2 (b)), corresponding to the C-C, C-N, C-O and C = O functions, respectively. MoO in FIG. 2 (c) 2 XPS fine spectra of N1 s for @ NHCS show four different types of nitrogen, pyridine N (398.3 eV), pyrrole N (399.9 eV), graphite N (401 eV) and oxidized N (402.6 eV). Comparison of XPS fine spectra of O1 s in FIG. 2 (d) revealed MoO 2 @ NHCS contains Mo-O (530.4 eV), C = O (531.22 eV), C = O (532.8 eV), and three oxygen-containing functional groups. XPS fine spectrum of Mo 3d (fig. 2 (e)) showed C = O containing Mo (IV) peaks at 232.6 eV and 235.7 eV, confirming MoO 2 Successful coupling.
To verify the MoO prepared by the method of the invention 2 How the @ NHCS nano material has the following properties is specially tested:
Pb 2+ removal performance testing
Under natural conditions, moO was studied 2 Application of @ NHCS as anode material in removing Pb in water body by capacitive deionization method 2+ The performance of (c).
The specific test method is as follows: 0.16g of MoO 2 @ NHCS, 0.02g conductive carbon black, 0.02g polyvinylidene fluorideMixing and stirring ethylene and N-dimethyl pyrrolidone for 24h to uniformly mix the slurry, taking a proper amount of slurry each time, coating the slurry on graphite paper, and wiping the graphite paper to 4 x 4cm to be used as a working electrode. In a 100mL beaker, 65mL of Pb (NO) at various concentrations 3 ) 2 In solution with MoO 2 The @ NHCS electrode is used as an anode, and the activated carbon electrode is used as a cathode for testing Pb under the conditions of different pH values and applied voltages 2+ The removal performance of (2).
As shown in fig. 4 (a), the effect at pH =3 to 8 was investigated, and the results showed Pb at pH =6 2+ The adsorption capacity is maximized. As shown in FIG. 4 (b), when the applied voltages were 0.6V, 0.8V, 1.0V, and 1.2V, pb was present as the applied voltage increased from 0.6V to 1.2V 2+ The adsorption capacity is higher and higher, and the adsorption capacity is maximum when the voltage is 1.2V. In conclusion, pb 2+ The best conditions for removal are: pH =6, applied voltage 1.2V. Then, under the optimum conditions, pb was tested 2+ The adsorption capacities at concentrations of 10, 30, 50, 80 and 100ppm, respectively, showed that the adsorption capacity increased with the increase in concentration.
To evaluate the stability of the material, one electrode was reused 20 times. As can be seen from FIG. 4 (d), the MoO load is 2 The electrode of @ NHCS has no obvious reduction in removal efficiency after being repeatedly used for 20 times, which indicates that the material has good cycle stability.
Claims (6)
1. MoO (MoO) 2 The preparation method of the @ NHCS hollow structure material is characterized by comprising the following steps: the method comprises the following steps:
a: firstly, intensively stirring a mixed solution containing tetraethyl silicate, ethanol, ammonia water and deionized water, then adding a dopamine hydrochloride solution into the mixed solution, stirring, centrifuging the mixed solution after the reaction is finished, and collecting a product SiO 2 @ PDA and washed, then dried;
b: prepared SiO 2 Calcining the @ PDA in nitrogen atmosphere to form nitrogen-doped silicon dioxide carbon spheres, dispersing the obtained product into hydrofluoric acid aqueous solution, continuously stirring, centrifugally collecting, and drying to obtain nitrogen-doped hollow carbon spheres;
c: dispersing ammonium molybdate into a mixed solvent of deionized water and ethylene glycol, adding the prepared nitrogen-doped hollow carbon spheres, performing ultrasonic treatment, pouring the mixture into a polytetrafluoroethylene-lined high-pressure reaction kettle for reaction, collecting and washing the obtained solid with deionized water and ethanol, and calcining the solid in a nitrogen atmosphere to obtain the molybdenum dioxide coupled nitrogen-doped hollow carbon spheres.
2. The MoO of claim 1 2 The preparation method of the @ NHCS hollow structure material is characterized by comprising the following steps: the preparation method comprises the following steps:
a: first, a solution containing 1mL of tetraethyl silicate, 24mL of ethanol, and 1mL of 28% NH was added 3 ·H 2 A mixed solution of O and 80mL of deionized water was vigorously stirred for 30min, and then 8mL and 50 mg. Multidot.mL were added -1 Adding the dopamine hydrochloride solution into the mixed solution, stirring for 24 hours, after the reaction is finished, centrifuging the mixed solution to collect a product, washing the product with deionized water and ethanol for several times, and collecting the obtained SiO 2 @ PDA, then dried at 80 ℃ for 24h;
b: prepared SiO 2 @ PDA at 800 ℃ at a temperature rise rate of 5 ℃/min, N 2 Calcining for 2 hours in the atmosphere to form nitrogen-doped silicon dioxide carbon spheres, dispersing the obtained product into 10wt% hydrofluoric acid aqueous solution, continuously stirring for 1 hour to completely remove silicon dioxide nuclei, centrifugally collecting, and drying at 80 ℃ to obtain nitrogen-doped hollow carbon spheres;
c: dispersing 0.3g of ammonium molybdate powder into a mixed solvent of 60mL of deionized water and 6mL of ethylene glycol, adding 0.06g of prepared nitrogen-doped hollow carbon spheres, carrying out ultrasonic treatment for 30min, pouring into a polytetrafluoroethylene lined high-pressure reaction kettle, heating for 10h at 150 ℃, collecting and washing the obtained solid with deionized water and ethanol, and then heating at 800 ℃ at a heating rate of 5 ℃/min and N 2 Calcining for 5 hours in the atmosphere to obtain the final product molybdenum dioxide coupled nitrogen doped hollow carbon spheres.
3. MoO (MoO) 2 The application method of the @ NHCS hollow structure material is characterized by comprising the following steps: adding MoO 2 @ NHCS hollow structure material as anode applied to capacitorRemoving lead ions by an ion method.
4. The MoO of claim 3 2 The application method of the @ NHCS hollow structure material is characterized by comprising the following steps: the method for removing lead ions by the capacitive deionization method comprises the following steps: adding MoO 2 Mixing and stirring the @ NHCS material, the conductive carbon black, the polyvinylidene fluoride and the N-methyl pyrrolidone uniformly, and MoO 2 The mass ratio of the @ NHCS material to the conductive carbon black to the polyvinylidene fluoride is 8:1:1, then coated on graphite paper as a working electrode, and charged with Pb (NO) containing solution in a beaker 3 ) 2 The solution is used for removing the Pb in the water body by applying working voltage by a blue battery testing system and performing liquid circulation by a peristaltic pump to perform a capacitance deionization method 2+ 。
5. The MoO of claim 4 2 The application method of the @ NHCS hollow structure material is characterized by comprising the following steps: method for removing Pb in water body by using capacitive deionization method 2+ In the process of (1), pb 2+ The concentration is 10-100 ppm; the pH value is 3-8; the applied voltage is 0.6-1.2V.
6. The MoO of claim 5 2 An application method of the @ NHCS hollow structural material is characterized in that: method for removing Pb in water body by capacitive deionization 2+ In the process of (1), pb 2+ The concentration is 10-100 ppm; the pH value is 6; the applied voltage was 1.2V.
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