CN111422840A - Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof - Google Patents
Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a phosphorus alkene/graphene three-dimensional aerogel material and a preparation method and application thereof, wherein graphene is prepared by a Hehm method, black phosphorus is prepared by a mineralization method, phosphorus alkene is prepared by a liquid phase intercalation method, then a certain amount of graphene and phosphorus alkene are uniformly dispersed in deionized water, ultrasonic stirring is carried out for a period of time, finally freeze drying is carried out, the phosphorus alkene and the graphene form a C-O-P bond and a C-P bond for self-assembly to obtain the phosphorus alkene/graphene three-dimensional aerogel material, the phosphorus alkene is applied to the treatment of uranium-containing radioactive wastewater, the phosphorus alkene/graphene three-dimensional aerogel material effectively reduces the degradation of the environment to the phosphorus alkene, improves the stability of the phosphorus alkene in the process of adsorbing and separating uranyl ions in the radioactive wastewater, improves the integral uranium adsorption capacity of the material, has extremely strong selectivity to the adsorption of uranium, and the preparation process is simple and controllable, has higher practical application value.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a phosphorus/graphene three-dimensional aerogel material and a preparation method and application thereof.
Background
Uranium is a radioactive element and is a main fuel of nuclear power, so that the main requirement for ensuring safe and efficient utilization of uranium is at present. A large amount of radioactive wastewater containing uranium, which contains uranium and spent fuel, is generated in the nuclear fuel circulation process of uranium ore mining, nuclear fuel processing, spent fuel treatment and disposal and the like226Ra、222Rn and210the decay daughter of Po and the like has chemical toxicity and radioactive toxicity, and if accumulated in a large amount in the environment, the decay daughter forms a potential threat to the survival of human beings and the development of environmental protection, so that the radioactive pollution abatement is one of the most challenging problems facing the present time. No matter the uranium is recycled from the uranium-bearing wastewater to improve the utilization rate of uranium resources or reduce the harm of radioactive wastewater to the environment, the uranium in the aqueous solution needs to be separated and enriched. Compared with common uranium separation and enrichment methods such as chemical precipitation, ion exchange, solvent extraction, filtration and reverse osmosis, the adsorption method has the advantages of wide material source, low cost, high selectivity, high speed, large capacity and the like, thereby being the most effective and common method for separating and enriching uranium from the environment.
The phosphorus alkene is single-layer or few-layer black phosphorus, is a novel two-dimensional material with a structure similar to graphene, and is formed by surrounding six P atoms into an annular hexagonal structure, and because of SP3The P atoms form a wrinkled surface structure by hybridization. The phosphorus alkene is another two-dimensional semiconductor material with a good application prospect after the graphene and the transition metal sulfide, and has a great application prospect in the fields of transistors, sensors, solar cells, electrode cells and the like. However, it also has a fatal problem that the phospholene is easily oxidized when exposed to the environmentDegradation, i.e. O in the environment under light conditions2Oxygen anions are formed on the surface of the phospholene and are gathered at the edge or the defect position, then the oxygen anions are combined with P atoms on the surface of the phospholene, and finally P-O is separated from the surface of the phospholene under the action of water molecules to form phosphoric acid, thereby causing the P-P bond on the surface of the phospholene to be broken. P at the fracture part is easy to combine with oxygen to form P-O, P-O is easy to combine with other P to form P-O-P, and P-O is easy to continuously separate from the surface of the phospholene under the action of water molecules, so the stability of the phospholene is extremely poor. Oxygen in P-O and P ═ O in the phosphate group is easy to complex with uranyl ions, and the phosphate group is often modified on the surfaces of various solid substrates and is used for adsorbing and separating the uranyl ions in radioactive wastewater. Therefore, the surface of the phosphorus alkene has rich P-O groups, and has good selective adsorption capacity on uranyl ions.
Therefore, the problem to be solved by the technical personnel in the field is how to improve the stability of the phosphenes in the environment and apply the phosphenes to the treatment of uranium wastewater.
Disclosure of Invention
In view of the above, the invention provides a phosphorus alkene/graphene three-dimensional aerogel material and a preparation method and application thereof, the graphene and phosphorus alkene are compounded, the environmental stability of the phosphorus alkene is effectively improved, and the phosphorus alkene is applied to uranium separation and enrichment, so that a good effect is achieved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a phosphorus/graphene three-dimensional aerogel material comprises the following steps:
(1) mixing red phosphorus, tin powder and tin iodide, filling the mixture into an ampoule bottle, vacuumizing until the pressure is less than 0.05Pa, sealing the ampoule bottle, heating the raw material end in the ampoule bottle to 200 ℃, then heating to 600 ℃, preserving heat for 6 hours, then cooling to 300 ℃, preserving heat for 2 days, and finally cooling to room temperature to obtain black product black phosphorus;
(2) weighing the black phosphorus prepared in the step (1), putting the black phosphorus into a test tube, dropwise adding N-methyl-2-pyrrolidone into the test tube, carrying out ultrasonic treatment at 40kHz for 24 hours, controlling the ultrasonic temperature to be less than or equal to 30 ℃, centrifuging to obtain a black solid at the bottom, and carrying out freeze drying to obtain phosphorus alkene;
(3) dispersing graphene oxide in deionized water to form a graphene aqueous solution; and (3) dispersing the phosphorus alkene prepared in the step (2) in deionized water to form a phosphorus alkene aqueous solution, mixing the phosphorus alkene aqueous solution and the deionized water, stirring for 3 hours, performing ultrasonic treatment at 30 ℃ and 40kHz for 3 hours, repeating the ultrasonic treatment for three times, and performing freeze drying to obtain the phosphorus alkene/graphene three-dimensional aerogel material.
Preferably, the mass ratio of the red phosphorus to the tin powder to the tin iodide in the step (1) is 50:2: 1.
Preferably, in the step (1), the temperature is raised to 600 ℃ for 1 hour, the temperature is lowered to 300 ℃ for 6 hours, and the temperature is lowered to room temperature for 10 hours after the temperature preservation at 300 ℃ is finished.
The principle of the preferred technical scheme is as follows: tin iodide and red phosphorus are completely sublimated to the upper part of the ampoule bottle at the temperature of 600 ℃, and the tin iodide cannot be decomposed due to the excessive existence of tin; then, in the cooling stage, tin iodide is firstly condensed and deposited at the bottom of the ampoule bottle to become a nucleation site of P; then, until about 300 ℃, P gas starts to grow at the nucleation site at the bottom, and the growth of the black phosphorus crystal is finished for about 10 hours.
Preferably, the ratio of the black phosphorus to the N-methyl-2-pyrrolidone in the step (2) is 1mg/m L.
The technical scheme has the advantages that the phosphorus alkene is stripped by using a liquid phase stripping method and using N-methyl-2-pyrrolidone, when the ratio of black phosphorus (g) to N-methyl-2-pyrrolidone (m L) is 5:1, the phosphorus alkene begins to be stripped, when the ratio of black phosphorus to N-methyl-2-pyrrolidone is smaller, the stripping effect and the stripping time are better, but when the ratio is smaller, the stripped lamella can be too small, and the protection is not facilitated.
The preparation method of the graphene oxide in the step (3) comprises the following steps:
(3.1) weighing graphite, adding a certain amount of a mixture of concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 3:1 to fully disperse the graphite to form graphite dispersion liquid of 2.5mg/m L mixed liquid, stirring for 24 hours, carrying out vacuum filtration, and drying to obtain a graphene interlaminar compound;
(3.2) heating the graphene interlayer compound prepared in the step (3.1) at 1000 ℃ for 10s to thermally expand the graphene interlayer compound to obtain expanded graphite;
(3.3) adding concentrated sulfuric acid and K into the expanded graphite powder prepared in the step (3.2)2S2O8And P2O5Stirring, heating at 80 ℃ for 5h, performing vacuum filtration, and drying to obtain pre-oxidized expanded graphite;
(3.4) placing the pre-oxidized graphite prepared in the step (3.3) in an ice water bath condition, adding concentrated sulfuric acid, and then adding KMnO4Then heated and stirred for 2H at 35 ℃ for dilution, and then 30% H is added2O2And standing, finally pouring out the supernatant, washing and purifying by using distilled water and hydrochloric acid solution, and drying to obtain the graphene oxide.
Preferably, the amount of concentrated sulfuric acid at 35 ℃ added in the step (3.3) is 60m L/g graphite, and the weight ratio of graphite to K is2S2O8：P2O5＝25:21:31。
Preferably, the concentrated sulfuric acid added in the step (3.4) is 40m L/g graphite, and the weight ratio of the graphite to the KMnO41:3, 30% H added2O2Was 2m L/g graphite.
Preferably, the concentration of the graphene aqueous solution in the step (3) is 0.1-10 mg/m L, and the concentration of the phosphorus aqueous solution is 1-5 mg/m L.
The beneficial effects of the preferred technical scheme are as follows: if the concentration of the phospholene aqueous solution is too low, it is easily oxidized excessively, and if it is too high, it is easily precipitated.
Preferably, the volume ratio of the graphene aqueous solution to the phosphorus aqueous solution is (1:100) - (100:1)
The beneficial effects of the preferred technical scheme are as follows: through adsorption experiments, graphene: the smaller the proportion of the phospholene (the more the phospholene content), the better the adsorption performance; however, when the mass percentage of the phosphorus is more than 20%, the film forming effect is poor, and the graphene cannot well protect the phosphorus.
The invention also provides the phosphorus alkene/graphene three-dimensional aerogel material prepared by adopting the technical scheme.
In addition, the invention also provides an application of the phosphorus/graphene three-dimensional aerogel material in uranium-containing wastewater treatment.
Preferably, the pH value of the uranium-containing wastewater is 3.0-5.5, the uranium concentration is 20-130 mg/L, and the treatment time is 130-180 min.
According to the technical scheme, compared with the prior art, the phosphorus/graphene three-dimensional aerogel material and the preparation method and application thereof disclosed by the invention have the following advantages:
the phosphorus alkene is applied to the treatment of the radioactive wastewater containing uranium, and the phosphorus alkene and the graphene are compounded to form a C-O-P bond and a C-P bond for self-assembly to prepare the phosphorus alkene/graphene three-dimensional aerogel material, so that the degradation of the phosphorus alkene by the environment is effectively reduced, and the stability of the phosphorus alkene in the process of adsorbing and separating uranyl ions in the radioactive wastewater is improved; moreover, the uranium adsorption capacity of the whole material is effectively improved by compounding the phosphorus/graphene material; the phosphorus/graphene composite two-dimensional material has strong selectivity on uranium adsorption by limiting the treatment conditions, and the preparation process is simple, convenient and controllable, and has high practical application value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an SEM and Mapping diagram of a three-dimensional phosphorus/graphene aerogel material;
FIG. 2 is a graph showing the stability of a phosphorus/graphene three-dimensional aerogel material;
FIG. 3 is a graph showing the influence of adsorption time on uranium adsorption of a phosphorus/graphene three-dimensional aerogel material when the initial uranium concentration is 50 mg/L and the pH is 5.5;
FIG. 4 is a graph showing the effect of uranium concentration on uranium adsorption of a phosphene/graphene three-dimensional aerogel material at a pH of 5.5;
FIG. 5 is a graph showing the effect of pH on uranium adsorption by a material;
FIG. 6 is a graph showing the amount of selective adsorption of materials at different pH;
FIG. 7 is a graph showing the selectivity of materials at different pH;
figure 8 is a graph showing the selective adsorption performance of the phosphorus/graphene three-dimensional aerogel material on uranium when the pH is 3.0.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Step one, preparation of graphene oxide
(3.1) weighing 5g of graphite, adding the graphite into a mixed solution of 150m L concentrated sulfuric acid and 50m L concentrated nitric acid, stirring for 24 hours, then carrying out vacuum filtration, and finally drying to obtain Graphene Interlaminar Compounds (GICs);
(3.2) heating the dried GICs powder at 1000 ℃ for 10 seconds to thermally expand it, thereby obtaining Expanded Graphite (EG);
(3.3) to the EG powder were added 300m L concentrated sulfuric acid, 4.2g K2S2O8And 6.2g P2O5Stirring and heating at 80 ℃ for 5h, then carrying out vacuum filtration, and drying to obtain pre-oxidized EG;
(3.4) to the pre-oxidized EG was added 200m L concentrated sulfuric acid followed by 15g KMnO under ice bath conditions4Heating and stirring for 2H at 35 ℃, diluting, and adding 10m L30% H30%2O2And standing for a period of time, pouring out the supernatant, washing and purifying by using distilled water and a hydrochloric acid solution, and drying to obtain the graphene oxide.
Step two, preparation of phosphorus alkene/graphite alkene three-dimensional aerogel material
(1) Mixing red phosphorus (500mg, 99.999%), tin powder (20mg, 99.999%) and tin iodide (10mg, 99%), filling the mixture into a quartz ampoule bottle, vacuumizing until the pressure is less than 0.05Pa, sealing the tube, heating the raw material end in the ampoule bottle to 200 ℃, then heating to 600 ℃ in 1h, preserving heat for 6h, then cooling to 300 ℃ in 6h, and preserving heat for 2 days. Finally, cooling to room temperature within 10h to obtain black product black phosphorus;
(2) weighing 10mg of black phosphorus, placing the black phosphorus in a test tube, dropwise adding 10m of L N-methyl-2-pyrrolidone (NMP), carrying out 40kHz ultrasonic treatment on the black phosphorus for 24 hours by using an ultrasonic cleaning machine, controlling the temperature to be not more than 30 ℃ by using a circulating water device during ultrasonic treatment, centrifuging to obtain black solid at the bottom, and carrying out freeze drying to obtain phosphorus alkene;
(3) dispersing the graphene oxide prepared in the step one in deionized water to form a graphene aqueous solution of 2.5mg/m L, dispersing the phosphorus prepared in the step 2 in deionized water to form a phosphorus aqueous solution of 2.5mg/m L, mixing the phosphorus aqueous solution and the phosphorus aqueous solution according to a volume ratio of 4:1, stirring for 3 hours, performing ultrasonic treatment at 30 ℃ and 40kHz for 3 hours, repeating the ultrasonic treatment for three times, and freeze-drying until ice cubes are completely sublimated, wherein the residue is the phosphorus/graphene three-dimensional aerogel material.
As shown in the attached drawing 1, the phosphorus alkene/graphene three-dimensional aerogel material is prepared by the technical scheme of the invention.
Test examples
Stability experiment of phosphorus alkene/graphene three-dimensional aerogel material
Weighing 10mg of phosphorus alkene/graphene three-dimensional aerogel material, putting the material into an aqueous solution with the pH value of 5.5, sealing, oscillating for 28 days, and measuring PO in the aqueous solution by using an ion chromatograph4The concentration, as shown in fig. 2, of the phosphorus/graphene three-dimensional aerogel material was reduced by 4% after immersion for 28 days in an aqueous solution with a pH of 5.5.
Second, static adsorption experiment
10mg of the phosphorus/graphene three-dimensional aerogel material is accurately weighed and placed in a conical flask with the thickness of 150m L, and then 50m L is added to fix the pH value (a certain amount of HNO is adopted)3Or NaOH regulated), the uranium solution with different initial concentrations at a solution temperature of 25 ℃ is put into a constant temperature shaking box, shaken for a period of time at 200rpm, and the supernatant is taken out and centrifuged. The uranium concentration in the solution is determined by using an ultraviolet spectrophotometry, the result is shown in the attached figure 3-5, and the phosphorus/graphene IIIThe adsorption capacity of the material to uranium is 453mg/g when the adsorption time of the material to uranium is 120min under the conditions that the pH value of the aerogel material is 5.5, the solution temperature is 25 ℃ and the initial concentration of a uranium solution is 50 mg/L, and the adsorption capacity of the material to uranium is 635mg/g when the adsorption time of the material to uranium is saturated under the conditions that the pH value of the aerogel material is 5.5, the solution temperature is 25 ℃ and the initial concentration of the uranium solution is 120 mg/L.
Third, selective adsorption experiment
Accurately weighing 10mg of the phosphorus/graphene three-dimensional aerogel material, adding the phosphorus/graphene three-dimensional aerogel material into a mixed solution of coexisting ions containing U (VI), Ce (III), Cs (I), Gd (III), L a (III), Sm (III), Co (II), Sr (II), Mn (II), Zn (II) and Ni (II) and having a predetermined pH value of 25m L, wherein the concentration of each ion is 0.5 mmol/L, centrifuging the mixed solution after constant-temperature oscillation for a period of time, collecting supernatant, and measuring the concentration of each ion in the liquid by using ICP-OES (inductively coupled plasma-optical storage system), wherein the result is shown in figures 6-8, and the total adsorption quantity q of the phosphorus/graphene three-dimensional aerogel material to metal ions ise(total)And adsorption capacity q of uraniume(U)The selectivity of the phosphorus/graphene three-dimensional aerogel material to uranium was the greatest at pH 5.0, 422mg/g and 231mg/g, respectively, and from the viewpoint of selectivity, the selectivity of the phosphorus/graphene three-dimensional aerogel material to uranium was the greatest at pH 3.0, 72%.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of a phosphorus/graphene three-dimensional aerogel material is characterized by comprising the following steps:
(1) mixing red phosphorus, tin powder and tin iodide, filling the mixture into an ampoule bottle, vacuumizing until the pressure is less than 0.05Pa, sealing the ampoule bottle, heating the raw material end in the ampoule bottle to 200 ℃, then heating to 600 ℃, preserving heat for 6 hours, then cooling to 300 ℃, preserving heat for 2 days, and finally cooling to room temperature to obtain black product black phosphorus;
(2) weighing the black phosphorus prepared in the step (1), putting the black phosphorus into a test tube, dropwise adding N-methyl-2-pyrrolidone into the test tube, performing ultrasonic treatment for 24 hours, controlling the ultrasonic temperature to be less than or equal to 30 ℃, centrifuging to obtain a black solid at the bottom, and performing freeze drying to obtain phosphorus alkene;
(3) dispersing graphene oxide in deionized water to form a graphene aqueous solution; and (3) dispersing the phosphorus alkene prepared in the step (2) in deionized water to form a phosphorus alkene aqueous solution, mixing the phosphorus alkene aqueous solution and the phosphorus alkene aqueous solution, stirring for 3 hours, performing ultrasonic treatment at 30 ℃ for 3 hours, repeating the ultrasonic treatment for three times, and performing freeze drying to obtain the phosphorus alkene/graphene three-dimensional aerogel material.
2. The preparation method of the phosphorus alkene/graphene three-dimensional aerogel material according to claim 1, wherein the mass ratio of red phosphorus to tin powder to tin iodide in the step (1) is 50:2: 1.
3. The preparation method of the phosphorus alkene/graphene three-dimensional aerogel material according to claim 1, wherein in the step (1), the temperature is raised to 600 ℃ for 1 hour, the temperature is lowered to 300 ℃ for 6 hours, and the temperature is lowered to room temperature for 10 hours after the temperature is maintained at 300 ℃.
4. The preparation method of the phosphorus/graphene three-dimensional aerogel material according to claim 1, wherein the ratio of black phosphorus to N-methyl-2-pyrrolidone in the step (2) is 1mg/m L.
5. The preparation method of the phosphorus alkene/graphene three-dimensional aerogel material according to claim 1, wherein the concentration of the graphene aqueous solution in the step (3) is 0.1-10 mg/m L, and the concentration of the phosphorus alkene aqueous solution is 1-5 mg/m L.
6. The preparation method of the phosphorus alkene/graphene three-dimensional aerogel material according to claim 1, wherein the volume ratio of the graphene aqueous solution to the phosphorus alkene aqueous solution is (1:100) - (100: 1).
7. The phosphorus/graphene three-dimensional aerogel material of any of claims 1-6.
8. Use of the phosphorus alkene/graphene three-dimensional aerogel material of claim 7 in uranium-containing wastewater treatment.
9. The application of the phosphorus/graphene three-dimensional aerogel material is characterized in that the pH of uranium-containing wastewater is 3.0-5.5, the uranium concentration is 20-130 mg/L, and the treatment time is 130-180 min.
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| CN111422840B (en) | 2022-12-13 |
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