CN115050586B - MXene nanosheet-aspergillus niger carbonized carbon composite material and preparation method and application thereof - Google Patents
MXene nanosheet-aspergillus niger carbonized carbon composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 241000228245 Aspergillus niger Species 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002135 nanosheet Substances 0.000 claims abstract description 18
- 239000002351 wastewater Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
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- 238000004108 freeze drying Methods 0.000 claims abstract description 6
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 4
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- VBWSWBQVYDBVGA-NAHFVJFTSA-N uranium-234;uranium-235;uranium-238 Chemical compound [234U].[235U].[238U] VBWSWBQVYDBVGA-NAHFVJFTSA-N 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 229920001817 Agar Polymers 0.000 description 3
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
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- LFGREXWGYUGZLY-UHFFFAOYSA-N phosphoryl Chemical group [P]=O LFGREXWGYUGZLY-UHFFFAOYSA-N 0.000 description 1
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/14—Fungi; Culture media therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/645—Fungi ; Processes using fungi
- C12R2001/66—Aspergillus
- C12R2001/685—Aspergillus niger
Abstract
The invention provides an MXene nanosheet-Aspergillus niger carbonized carbon composite material, and a preparation method and application thereof, wherein the preparation method comprises the following steps: step 1, adding MXene nano-sheets and a pH buffer solution into water, uniformly mixing, adding aspergillus niger, uniformly mixing, culturing, and freeze-drying a solid product obtained by culturing to obtain a precursor; step 2, annealing the precursor at 650-850 ℃ to obtain carbide; step 3, activating the carbide to obtain an MXene nanosheet-Aspergillus niger carbonized carbon composite material; the MXene-Aspergillus niger carbonized carbon composite structure can be used as an electrode material for purifying the capacitive deionized nuclear wastewater, and the adsorption efficiency of radioactive ions in water is greatly improved.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to an MXene nanosheet-Aspergillus niger carbonized carbon composite material, and a preparation method and application thereof.
Background
Nuclear energy has various advantages, but the large amount of waste generated thereby also greatly limits the rapid development of nuclear energy. The radioactive elements enter the water body to cause radioactive pollution. Radioactive wastewater refers to wastewater discharged from nuclear fuel pretreatment and post-treatment, nuclear power plants, research using radioactive isotopes, hospitals, factories, and the like. Uranium-containing wastewater is a widely-available radioactive wastewater such as uranium mining and hydrometallurgy wastewater, uranium refining and nuclear fuel manufacturing wastewater, reactor operation wastewater, post-treatment wastewater of reactor fuel, wastewater generated by radioisotope production, and wastewater generated by factories and research departments using radioisotope, etc., and mainly comprises uranium 238 UO 2 2+ ) Laser @ 225 Ra 2+ ) The iodine is 131/129/125 I - ) Cesium [ ] 137 Cs + ) And plutonium # - 239 /240/241 Pu 4+ ) And isopolynuclide ions.
The water body can cause the change of characteristics in chemical, physical, biological or radioactive aspects due to the intervention of the elements, thereby affecting the effective utilization of the water, endangering the health of human bodies or damaging the ecological environment and causing the phenomenon of water quality deterioration. At present, 70% of the earth surface is covered by water, but the available fresh water resource of human beings is less than 1%, the fresh water resource is a subject which is often polluted by human activities, and the polluted water body is very difficult to recover, so that the research and development of the efficient, environment-friendly and low-cost nuclear waste liquid treatment technology has great social, economic and environmental significance for reducing the pollution of radioactive wastewater to the environment.
The main processes of the current water purification technology for removing radioactive substances are a coagulation method, an adsorption method, an ion exchange method and a biological treatment method. In the conventional treatment method, different defects such as simple process and low cost of a coagulating sedimentation method exist, but sediment products are not easy to enrich and recycle and secondary pollution is easy to cause; the evaporation concentration method is simple and effective, has high removal rate, but has higher cost; the extraction method has good effect, low concentration of uranium removal but high treatment cost, and large amount of waste residues after extraction; the uranium removal rate of the reverse osmosis method is high, but the treatment cost is high and the industrial application is difficult. The traditional biological treatment method is widely applied due to the characteristics of wide material sources, various varieties, high selectivity and low cost, but the adsorption efficiency of the biological treatment method is not high.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an MXene nanosheet-Aspergillus niger carbonized carbon composite material, and a preparation method and application thereof, wherein the MXene-Aspergillus niger carbonized carbon composite structure can be used as an electrode material for purifying the capacitive deionized nuclear wastewater, and the adsorption efficiency of radioactive ions in water is greatly improved.
The invention is realized by the following technical scheme:
the invention firstly selects aspergillus niger spores with strong radiation resistance, strong vitality and strong uranium removal capability for cultivation improvement, then prepares the MXene nano-sheets, and then prepares the composite structure of aspergillus niger and the MXene nano-sheets, so that the two-dimensional nano-channel provides a rapid ion migration path, and optimizes specific capacitance and multiplying power performance. Then through annealing and activation, the specific surface area of the materials is further increased, and finally, the electrode film is prepared for purifying nuclear wastewater.
The preparation method of the MXene-Aspergillus niger carbonized carbon composite structure comprises the following steps:
(1) Screening to obtain Aspergillus niger from soil, performing pure seed separation, bevel activation, and performing mutation breeding on Aspergillus niger strains by using 2kGy gamma rays; thus, aspergillus niger spores can be prepared
(2) Ti is added at room temperature 3 AlC 2 Soaking the powder in an etching solution for etching, and performing ultrasonic treatment to obtain a suspension;
(3) Centrifuging the suspension, repeatedly cleaning with deionized water until the solution is neutral, and centrifuging to obtain precipitate (Ti) 3 C 2 T X ；
(4) Ti is mixed with 3 C 2 T X Mixing with DMSO and stirring at room temperature, and centrifuging the mixed solution to obtain precipitate;
(5) Precipitate the precipitateAnd H 2 Mixing and ultrasonic treating at room temperature, centrifuging the dispersion liquid obtained by ultrasonic treating, and vacuum filtering the supernatant liquid with a polypropylene filter membrane;
(6) Airing the filter cake at room temperature to obtain layered Ti 3 C 2 T X Thus, an MXene nanoplatelet was prepared.
(7) Adding peptone and glucose into distilled water according to the proportion of 1000mL of water of 16-20 g of peptone and 20-25 g of glucose, uniformly stirring, heating and boiling for 20-30 min for disinfection, so that the peptone and the glucose are completely dissolved;
(8) Sealing and fixing the solution obtained in the step (7) by using a sealing film, performing ultrasonic treatment, and then placing the solution into a high-temperature sterilization pot at 100-125 ℃ for sterilization for 15-50 min, thereby preparing a liquid culture medium of aspergillus niger;
(9) Inoculating Aspergillus niger spores on a liquid culture medium, culturing for 3-5 days in an incubator at the temperature of 30-35 ℃ to obtain spherical Aspergillus niger balls, and cleaning the Aspergillus niger balls to obtain Aspergillus niger;
(10) Adding a certain amount of MXene nano-sheets, citric acid with the mass fraction of 0.05-0.1% and 1-2% sodium citrate aqueous solution into distilled water, stirring for 10-20 minutes, performing ultrasonic treatment, and after the solution is mixed for a certain time, mixing the aspergillus niger obtained by culturing in a liquid nutrient medium with the prepared mixed solution in a ratio of 10-20 g: mixing 1000mL, stirring, culturing at 35deg.C for 1-2 days, and placing the dehydrated thallus into a medium containing CaCl 2 Storing the drying agent in a drying box for standby;
(11) Putting the dehydrated thalli in the step (10) into a freeze drying agent for freeze drying;
(12) Drying and then placing the mixture into a tubular furnace, heating the mixture to 650-850 ℃ and preserving heat for 3-5 hours to obtain MXene nanosheets-Aspergillus niger carbides;
(13) Uniformly mixing the MXene nanosheet-Aspergillus niger carbide obtained in the step (12) and potassium hydroxide according to the mass ratio of 1:3-5, and then placing the mixture into a tube furnace at the temperature of 1-3 ℃ for min -1 Heating to 600-900 deg.C, preserving heat for 2-5 h, cooling, preparing hydrochloric acid solutionRepeatedly cleaning, washing with absolute ethyl alcohol and deionized water until the pH value is 7, and then putting into an oven for drying to obtain the MXene nano-sheet-aspergillus niger composite material.
The method for preparing the electrode by adopting the MXene nanosheet-Aspergillus niger composite material as an electrode material comprises the following steps:
1) Pouring a proper amount of polyvinylidene fluoride (PVDF) into N-methyl pyrrolidone (NMP), and fully stirring until the PVDF is completely dissolved;
2) Adding a proper amount of Super P Li into the solution obtained in the step 1), and continuing to stir for 1-5 h with strong force;
3) Adding MXene nanosheet-Aspergillus niger composite powder, and stirring strongly to obtain uniformly mixed electrode slurry;
4) And uniformly coating the mixed slurry on the surface of the aluminum foil by using a coating machine, and primarily drying at 120-150 ℃. The height of a scraper of the coating machine is controlled to obtain a coating with the thickness of 10-100 micrometers;
5) And then the uncleaved aluminum foil pole piece obtained in the step 4) is subjected to pressurizing treatment for 30-120 s under 10-30 MPa, the size of the electrode is cut according to the size, and the electrode is placed into a vacuum drying oven for vacuum drying for 16-48 h, so that the electrode is prepared.
Compared with the prior art, the invention has the following beneficial effects:
the invention enriches MXene on aspergillus niger, combines groups such as-OH, -F and the like which are rich on the surface of the MXene and are easy to combine with heavy metal ions with surface functional groups such as hydroxyl, carboxyl, phosphoryl and the like on the surface of fungal cells to form a stable composite structure system, and obtains the MXene-aspergillus niger carbonized carbon composite material through annealing and activation, thereby combining the MXene and the aspergillus niger carbonized carbon to form a composite structure. Similar to graphene, MXene has higher specific surface area, excellent flexibility, good hydrophilicity and conductivity, and unique component diversity, layer thickness controllability and structure adjustability, when the MXene nano-sheet is used as an electrode material for purifying the capacitance deionized nuclear wastewater, the MXene nano-sheet can be used as an effective conductive layer, the high conductivity of MXene is utilized, a quick ion migration path is provided by the two-dimensional nano-channel of MXene,the specific capacitance and the multiplying power performance are optimized, the mass specific capacitance can reach 499F/g at room temperature, and the composite conductivity is increased, so that the efficiency of electrochemical reaction is improved, and a strong pseudo-capacitance effect is generated. In addition, the MXene nano-sheet can also be used as a stabilizer with a complex mixed structure, so that the stacking and aggregation processes are prevented, the cycling stability of the electrode material is improved, in addition, the MXene nano-sheet can also be used as a curing additive for treating radioactive waste liquid, and the leaching rate of the radionuclide is reduced. Aspergillus niger is a biological strain with high radiation resistance, strong viability and strong uranium removal property, and the saturated adsorption capacity of the Aspergillus niger to radioactive uranium element is 60-80 mg/g. The biomass carbon derived from the biomass carbon has rich macroporous-microporous-mesoporous structure (specific surface area is as high as (2230 m 2 Pore size distribution (3-4 nm)), one-dimensional fiber shape, abundant surface defects and active point positions, nitrogen element doping and the like, the saturated adsorption capacity of the nano-composite material on radioactive elements is obviously higher than that of active carbon common in the market (the adsorption capacity of uranium ions can reach 46.83mg/g, and the specific capacity is 194F/g. Meanwhile, compared with commercial carbon particles, the strain has one-dimensional fiber shape, so that the strain has good electrical property, is more beneficial to current transportation, and can remarkably improve the electrochemical adsorption property of a composite structure. The invention can realize the synergistic enhancement effect of the specific capacitance of the fungal carbon and MXene, perfectly solve the defects of lower capacitance capability of the fungal (poor mechanical strength) and the existing carbon-based electrode active material, poorer cycling stability of the metal oxide electrode material and the like, and improve the adsorption capability of the fungal carbon to radioactive uranium elements. The preparation method is simple and has low cost.
Furthermore, the mass ratio of the MXene nano-sheet to the Aspergillus niger can ensure that the adsorption performance can reach the optimal effect.
Furthermore, after the Aspergillus niger spores are subjected to mutagenesis treatment by adopting gamma rays, the strain has the characteristics of long service life, strong uranium removal capability and radiation resistance.
Furthermore, the activation temperature of the invention can enlarge the specific surface area of aspergillus niger to the greatest extent, and does not damage the structure of the aspergillus niger. If the activation temperature is too high, adsorption becomes particularly slow, affecting its adsorption properties.
The MXene nanosheet-Aspergillus niger carbonized carbon composite material prepared by the method has the characteristics of unique one-dimensional tubular structure, high specific surface area, high conductivity, uniform pore size distribution and the like, is used as an electrode material for purifying nuclear wastewater by a capacitive deionization method, and the unique composite structure after carbonization can further improve the adsorption capacity of the composite material by selective adsorption, solidification and other effects on target nuclear ions through selective and synergistic effects, so that radioactive elements in nuclear polluted water bodies can be adsorbed and removed with high efficiency and high selectivity, the saturated adsorption capacity of the composite material on radioactive uranium elements is about 110mg/g, and the composite material can be recycled. The whole nuclear wastewater purification process is simple, the purification time is short, the cost is low, an ion exchange membrane is not needed, and the radioactive ions in water can be removed more efficiently, so that the method is a nuclear wastewater treatment method with great development prospect.
Drawings
FIG. 1 is an SEM image of the cultured Aspergillus niger of example 1 of the present invention at various magnifications;
FIG. 2 shows a strain cultivation process in example 1 of the present invention;
FIG. 3 is a photograph showing the growth of strains in example 1 of the present invention;
FIG. 4 is capacitive deionization adsorption data for example 1 of the present invention;
FIG. 5 is an SEM image of an MXene nanoplatelet according to example 1 of the invention;
FIG. 6 is an electron microscope scan of the MXene nanoplatelets of example 1 of the present invention after being compounded with Aspergillus niger species;
FIG. 7 is a schematic diagram of a combined flow path of MXene and Aspergillus niger in the present invention.
Detailed Description
For a further understanding of the present invention, the present invention is described below in conjunction with the following examples, which are provided to further illustrate the features and advantages of the present invention and are not intended to limit the claims of the present invention.
Example 1: carbon carbide and Ti based on Aspergillus niger 3 C 2 T X Method for purifying capacitor deionized nuclear wastewater
(1) The method comprises the steps of selecting about 10g of mould humus with good growth vigor of mould from underground storage of nuclear reactor spent fuel of Russian Tomsk university, screening out Aspergillus niger strains, and dissolving 10g of peptone, 5g of yeast extract, 10g of sodium chloride and 10.8g of agar powder in 0.9L of water by adopting an agar medium. Adding calcium carbonate, selecting colony with large transparent ring from the grown colony on the inclined plane, selecting Aspergillus niger strain with strong uranium removing performance from the colony, inoculating the strain to the inclined plane for activation, adding a small amount of sterile distilled water into an agar inclined plane culture medium, scraping fresh mould spores on the surface by using a sterile inoculating loop, placing the spore suspension into a 250mL cone flask, and injecting 40mL eluent. Then adding 12 glass beads with the diameter of 5mm into a conical flask, mixing with spores, putting into a water area oscillator, vibrating and dispersing the spores, and filtering by using a single-layer cotton gauze to remove hyphae. Then loading into a sterilizing centrifuge tube to separate precipitated spores, removing supernatant, adding 40mL of eluent, and repeating centrifugation operation for 3 times to obtain 10 6 Spores/mL of mould spore suspension. Finally, carrying out mutagenesis treatment by using gamma rays with the dosage of 2kGy, then separating spores subjected to the mutagenesis treatment by using a plate added with calcium carbonate, selecting 200 single colonies with larger transparent circles after colony growth, and culturing and growing Aspergillus niger spores at the temperature of 30 ℃; then Ti is added at room temperature 3 AlC 2 Soaking the powder in 50% hydrofluoric acid solution for 2 hr, ultrasonic treating to obtain suspension, repeatedly cleaning with deionized water until the solution is neutral, and centrifuging to obtain precipitate Ti 3 C 2 T X The method comprises the steps of carrying out a first treatment on the surface of the And then Ti is added 3 C 2 T X Mixing with DMSO at a mass ratio of 1:20, stirring at room temperature for 18h, and centrifuging at 3500rpm for 20min to obtain precipitate; precipitate and H 2 O is mixed in a mass ratio of 1:500 and is sonicated for 4 hours at room temperature by 300W, then the dispersion liquid obtained by the sonication is centrifuged for 10 minutes at 2000rpm, the obtained supernatant is vacuum filtered by a polypropylene filter membrane, and the layering Ti is obtained by airing and suction filtration at room temperature 3 C 2 T X 。
(2) Peptone and glucose were purchased in the market, 16g peptone and 20g glucose were added to 1000mL distilled water and dissolved in a conical flask, stirred well, boiled for 26min and sterilized, so that peptone and glucose were completely dissolved. Then wrapping with sealing film, fixing with rubber band, placing in an ultrasonic machine, ultrasonic treating for 10min, dispersing uniformly, heating in a high-temperature sterilizing pan at 121deg.C for 15min, closing the high-temperature sterilizing pan, taking out the conical flask, and rapidly moving onto an ultra-clean workbench. When the conical flask was cooled to near room temperature, the prepared liquid culture medium was dispensed into 50mL conical flasks in an amount of 30mL each in a sterile room, and sealed with a culture membrane;
(3) Inoculating Aspergillus niger spores directly on a liquid culture medium in an ultra-clean laboratory by using an inoculating gun head, culturing for 4 days at 35 ℃ in an incubator, obtaining small spherical fungus balls in a conical flask, then pouring out redundant nutrient solution in the conical flask, and cleaning with distilled water to obtain Aspergillus niger (the strain is Aspergillus niger Multishot 550, and is preserved in China industry microbiological culture collection center, and the preservation number is CICC 2487);
(4) A certain amount of MXene nano-sheets and 25mL of citric acid with mass fraction of 0.1% and 2% sodium citrate aqueous solution are added into 1000mL of distilled water, stirred for 5 minutes and treated by ultrasonic for 15 minutes to obtain a mixed solution, and aspergillus niger and the prepared mixed solution are mixed according to 20g:1000mL (the mass ratio of MXene nanosheets to aspergillus niger is 1:3), stirring uniformly, then continuously culturing for 2 days at 35 ℃, and finally placing the obtained dehydrated thalli into a medium with CaCl 2 And (5) storing the drying agent in a drying box for later use.
(5) Placing dehydrated Aspergillus niger in a freeze drying agent for freeze drying, placing in a tube furnace, heating to 750deg.C, and maintaining for 3 hr to obtain carbide, mixing the carbide and potassium hydroxide at a mass ratio of 1:4, and placing in the tube furnace at 3deg.C for 3 min -1 Heating to 800 ℃ at the heating rate, preserving heat for 2 hours, cooling, preparing 60ml of hydrochloric acid for repeated cleaning, washing by absolute ethyl alcohol and deionized water until the pH value is=7, and then putting into an oven for drying; obtaining the MXene nanosheet-Aspergillus niger carbonized carbon composite material.
(6) Then a proper amount of polyvinylidene fluoride (PVDF) is poured into N-methyl pyrrolidone (NMP) and is fully stirred until PVDF is completely dissolved, and then a proper amount of PVDF is addedContinuously and strongly stirring for 1h, then adding MXene nano-sheet-Aspergillus niger carbonized carbon composite material powder, and strongly stirring for 3h to obtain uniformly mixed ground electrode slurry, wherein the mass ratio of the MXene nano-sheet-Aspergillus niger carbonized carbon composite material to PVDF is 90:5:5, and the solid content of the slurry is 25%; then the mixed sizing agent is evenly coated on the surface of the aluminum foil by a coating machine, and the tape feeding speed is 6 m.min -1 The primary drying temperature is 120 ℃. The height of a scraper of a coating machine is controlled to obtain a coating with 88 mu m, and the obtained pole piece is subjected to pressurizing treatment for 30 seconds under 10 MPa; then sizing the electrodes according to the size; finally, the mixture is placed into a vacuum drying oven for vacuum drying at 200 ℃ for 16 hours.
Example 2: carbon carbide and Ti based on Aspergillus niger 3 C 2 T X Method for purifying capacitor deionized nuclear wastewater
The same as in example 1, except that the etching liquid hydrofluoric acid was replaced with LiF/HCl mixed liquid in step (1).
Example 3: carbon carbide and Ti based on Aspergillus niger 3 C 2 T X The method for purifying the capacitive deionization nuclear wastewater of (2) is the same as in example 1, except that in step (1), the etching liquid hydrofluoric acid is replaced with NH 4 HF 2 A solution.
FIG. 1 shows the cultured Aspergillus niger in example 1 of the present invention, and shows that the strain has a one-dimensional fibrous structure.
FIG. 2 shows the strain cultivation process in example 1 of the present invention, and FIG. 3 shows the strain growth picture. FIG. 4 is a graph of capacitance deionized data in example 1 of the present invention, and the specific capacitance is calculated by the I-V graph, and from FIG. 4, it can be calculated that the specific capacitance of the composite material prepared in example 1 of the present invention can reach 499F/g, the saturated adsorption capacity for radioactive uranium element is about 110mg/g, and is significantly higher than the adsorption capacity of Aspergillus niger of 60-80 mg/g.
FIG. 5 is an electron microscope image of the MXene nanoplatelets prepared in example 1 of the present invention, it can be seen that Ti 3 C 2 T x The thickness of the single-layer nano-sheet is about 1nm, and the nano-sheet is relatively flat and has no hollow.
FIG. 6 is an electron microscope scan of the MXene nanoplatelets of example 1 of the present invention after complexing with Aspergillus niger species, which can be seen to be distributed on the MXene nanoplatelets.
FIG. 7 is a schematic illustration of a composite flow of MXene nanoplatelets and Aspergillus niger species, few-layered Ti being obtained by ultrasonic stripping 3 C 2 T x Then forming MXene nano-sheets by layer-by-layer self-assembly, and compositing with Aspergillus niger strains while layer-by-layer self-assembly.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (5)
1. The preparation method of the MXene nanosheet-Aspergillus niger carbonized carbon composite material is characterized by comprising the following steps of:
step 1, adding MXene nano-sheets and a pH buffer solution into water, uniformly mixing, adding aspergillus niger, uniformly mixing, culturing, and freeze-drying a solid product obtained by culturing to obtain a precursor; the mass ratio of the MXene nano-sheet to the aspergillus niger is 1:3; the pH buffer solution is citric acid with mass fraction of 0.05-0.1% and sodium citrate aqueous solution with mass fraction of 1-2%;
step 2, annealing the precursor at 650-850 ℃ to obtain carbide;
step 3, mixing carbide and potassium hydroxide, heating to 600-900 ℃, preserving heat for 2-5 hours, and washing the obtained product to obtain the MXene nanosheet-Aspergillus niger carbonized carbon composite material;
in the step 1, the preparation method of the aspergillus niger comprises the following steps:
performing mutagenesis treatment on the aspergillus niger spores by adopting gamma rays, and then inoculating the mutagenized aspergillus niger spores on a liquid culture medium for culturing to obtain the aspergillus niger;
in the step 1, the preparation method of the MXene nano-sheet comprises the following steps:
ti is mixed with 3 AlC 2 Soaking the powder in an etching solution for etching to obtain a suspension;
centrifuging the suspension, washing the obtained solid with deionized water until the washing liquid is neutral to obtain Ti 3 C 2 T X ；
Ti is mixed with 3 C 2 T X Stirring and mixing with DMSO, and centrifuging the obtained mixed solution to obtain a precipitate;
and (3) ultrasonically mixing the precipitate with water, centrifuging a dispersion liquid obtained by ultrasonic treatment, vacuum-filtering the obtained supernatant with a polypropylene filter membrane, and drying to obtain the MXene nano-sheet.
2. The MXene nanosheet-Aspergillus niger carbonized carbon composite material obtained by the preparation method of claim 1.
3. An electrode characterized in that the electrode surface is covered with an electrode film comprising the MXene nanoplatelet-aspergillus niger carbonized carbon composite of claim 2.
4. A capacitive deionization device comprising the electrode of claim 3.
5. The TiO according to claim 2 2 -use of an aspergillus niger carbonized carbon composite, an electrode according to claim 3 or a capacitive deionization device according to claim 4 for the purification of nuclear wastewater by capacitive deionization.
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