CN105854913A - Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof - Google Patents
Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof Download PDFInfo
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- CN105854913A CN105854913A CN201610212655.4A CN201610212655A CN105854913A CN 105854913 A CN105854913 A CN 105854913A CN 201610212655 A CN201610212655 A CN 201610212655A CN 105854913 A CN105854913 A CN 105854913A
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- 239000000126 substance Substances 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 41
- 239000002184 metal Substances 0.000 title claims abstract description 41
- 239000011858 nanopowder Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007864 aqueous solution Substances 0.000 claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000919 ceramic Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 4
- 239000011941 photocatalyst Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 150000001722 carbon compounds Chemical class 0.000 claims description 49
- 239000000203 mixture Substances 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 5
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 4
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 3
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 239000012448 Lithium borohydride Substances 0.000 claims description 2
- NGIISMJJMXRCCT-UHFFFAOYSA-N [Ru].[N+](=O)(O)[O-] Chemical compound [Ru].[N+](=O)(O)[O-] NGIISMJJMXRCCT-UHFFFAOYSA-N 0.000 claims description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 229940097267 cobaltous chloride Drugs 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 2
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229940078494 nickel acetate Drugs 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims description 2
- RWRDJVNMSZYMDV-UHFFFAOYSA-L radium chloride Chemical compound [Cl-].[Cl-].[Ra+2] RWRDJVNMSZYMDV-UHFFFAOYSA-L 0.000 claims description 2
- 229910001630 radium chloride Inorganic materials 0.000 claims description 2
- VXNYVYJABGOSBX-UHFFFAOYSA-N rhodium(3+);trinitrate Chemical compound [Rh+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VXNYVYJABGOSBX-UHFFFAOYSA-N 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 10
- 239000002244 precipitate Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 239000010865 sewage Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 239000010931 gold Substances 0.000 description 7
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 238000013019 agitation Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 229910009818 Ti3AlC2 Inorganic materials 0.000 description 3
- 238000002372 labelling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 229910003178 Mo2C Inorganic materials 0.000 description 1
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 description 1
- 229910004472 Ta4C3 Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2101/30—Organic compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention relates to two-dimension carbide loaded metal simple substance nano-powder, and a preparation method and an application thereof. The preparation method comprises the following steps: (1) soaking MAX phase ceramic powder in a hydrochloric acid solution in which lithium fluoride is dissolved, stirring, centrifugally separating, washing with deionized water and ethyl alcohol, drying and then acquiring solid powder, namely, two-dimension carbide; (2) dissolving the two-dimension carbide in a metal saline solution and preparing into a mixing solution; (3) adding a reducing agent aqueous solution into the mixing solution while stirring, reacting for 0.5-2h at room temperature, and washing and drying the solid precipitate acquired by centrifuging the turbid liquid after ending the reaction, thereby acquiring the two-dimension carbide loaded metal simple substance nano-powder. According to the invention, the uniform loading of metal simple substance nano-particles on the surface of the two-dimension carbide and between the layers is realized; according to the method, various metal simple substance nano-particles are loaded onto the two-dimension carbide; the prepared two-dimension carbide loaded metal simple substance nano-powder as a photocatalyst has excellent application prospect in the field of treating organic pollutants in sewage.
Description
Technical field
The invention belongs to nano composite material preparation field, be specifically related to a kind of Two-dimensional Carbon compound carried metal simple substance nano-powder, preparation method and applications.
Background technology
MXene is a kind of New Two Dimensional carbide nanometer material with class graphene-structured, the transition metal carbide obtained by active metal layer " A " element of hf etching ternary layered ceramic MAX phase or carbonitride, study widely owing to its special physico-chemical property causes in recent years.Up to now, MXene family includes: Ti3C2、Ti2C、V2C、Nb2C、Mo2C、(Ti0.5Nb0.5)2C、Ti3CN、(V0.5Cr0.5)3C2, and Ta4C3
Have Deng, MXene and be similar to the two-dimensional slice structure of Graphene and bigger specific surface area, many technical fields such as absorption, catalysis, ultracapacitor, lithium ion battery, sensor can be widely used in.
In prior art, the work of research is mainly the load of aspect performance, little study two-dimensional carbide nanometer material and the metal simple-substance nano-particle such as MXene one-component and the absorption of load oxidate nano composite [ZL201410137498.6], lithium electricity and ultracapacitor.
Summary of the invention
It is an object of the invention to provide a kind of Two-dimensional Carbon compound carried metal simple substance nano-powder, preparation method and applications.
Based on above-mentioned purpose, the present invention adopts the following technical scheme that:
The preparation method of a kind of Two-dimensional Carbon compound carried metal simple substance nano-powder, comprises the steps:
(1) being immersed in the hydrochloric acid solution being dissolved with lithium fluoride by MAX phase ceramics powder, stirring, centrifugation, successively with deionized water and ethanol purge, dried gained pressed powder is Two-dimensional Carbon compound (i.e. MXene)；
(2) Two-dimensional Carbon compound (i.e. MXene) being dissolved in aqueous metal salt and make blend solution, the Two-dimensional Carbon compound (i.e. MXene) concentration in blend solution is 8 ~ 10g/L；
(3) under stirring, reducing agent aqueous solution is joined in above-mentioned blend solution, reducing agent aqueous solution is 1 (1-1.2) with the volume ratio of blend solution, room temperature reaction 0.5-2h, after reaction terminates, being centrifuged by gained suspension, gained solid precipitation washs, is drying to obtain Two-dimensional Carbon compound carried metal simple substance nano-powder.
Further, described Two-dimensional Carbon compound is Ti3C2、Ti2C or V2C。
Slaine in aqueous metal salt is at least one in silver nitrate, gold chloride, chloroplatinic acid, Palladous chloride., Palladous nitrate., radium chloride, rhodium nitrate, ruthenic chloride, nitric acid ruthenium, iron chloride, ferric nitrate, iron sulfate, cobaltous chloride, cobalt nitrate, cobalt acetate, cobaltous sulfate, Nickel dichloride., nickel nitrate, nickel sulfate, nickel acetate, copper chloride, copper nitrate, copper sulfate and copper acetate, and the concentration of aqueous metal salt is 0.01-0.1mol/L.
Reducing agent in reducing agent aqueous solution is NaBH4、KBH4、LiBH4, one or more combination in hydrazine hydrate and sodium citrate, and the concentration of reducing agent aqueous solution is 0.05-0.1mol/L.
Use the Two-dimensional Carbon compound carried metal simple substance nano-powder obtained by above-mentioned preparation method.
The application in terms of photocatalytic degradation dirt organic pollutants of the above-mentioned Two-dimensional Carbon compound carried metal simple substance nano-powder.
The preparation method of Two-dimensional Carbon compound carried metal simple substance nano-powder of the present invention need not add any catalyst, and content of metal is adjustable, and reaction can be carried out at different temperatures, and reaction condition is gentle.Present invention process method is simple, with low cost, without special process equipment, convenience and high-efficiency, achieve metal simple-substance nano-particle in MXene surface and the uniform load of interlayer, the method can load various metals simple substance nano-particle to MXene, and prepared Two-dimensional Carbon compound carried metal simple substance nano-powder has a good application prospect processing dirty organic pollutants field as photocatalyst.
Accompanying drawing explanation
Fig. 1 is the field emission scanning electron microscope photo of the Two-dimensional Carbon compound MXene load simple substance Ag nano-powder of the embodiment of the present invention 1 preparation；
Fig. 2 is Two-dimensional Carbon compound MXene and the X ray diffracting spectrum of load simple substance Ag nano-powder thereof of the embodiment of the present invention 1 preparation；
Fig. 3 is the field emission scanning electron microscope photo of the Two-dimensional Carbon compound MXene load simple substance Au nano-powder of the embodiment of the present invention 2 preparation；
Fig. 4 is Two-dimensional Carbon compound MXene and the X ray diffracting spectrum of load simple substance Au nano-powder thereof of the embodiment of the present invention 2 preparation；
Fig. 5 is the field emission scanning electron microscope photo of the Two-dimensional Carbon compound MXene load simple substance Pd nano-powder of the embodiment of the present invention 3 preparation；
Fig. 6 is Two-dimensional Carbon compound MXene and the X ray diffracting spectrum of load simple substance Pd nano-powder thereof of the embodiment of the present invention 3 preparation；
Fig. 7 is the photocatalysis performance test result of Two-dimensional Carbon compound MXene carried metal nano-powder prepared by the present invention, and photocatalytic degradation efficiency uses methylene blue equilibrium concentration (C after ultraviolet lightingt) with illumination before methylene blue initial concentration (C0) percent of ratio represents.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described in further details, but protection scope of the present invention is not limited thereto.
Embodiment 1:
Its preparation method of a kind of Two-dimensional Carbon compound carried metal simple substance Ag nano-powder, comprises the steps:
(1) by 5g MAX phase Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M being dissolved with 5g lithium fluoride, magnetic agitation 48h at a temperature of 40 DEG C, centrifugation precipitates, clean to using washes of absolute alcohol again three times close to neutrality through deionized water, being vacuum dried 12h at a temperature of being deposited in 80 DEG C, gained pressed powder is Two-dimensional Carbon compound；
(2) weighing 0.1g silver nitrate to be dissolved in 50 mL deionized waters, room temperature stirs evenly；It is dispersed in above-mentioned silver nitrate aqueous solution make blend solution by 0.5g Two-dimensional Carbon compound pressed powder, stirs；
(3) with vigorous stirring by the NaBH of 50mL 0.1mol/L4Aqueous solution is slowly added in the blend solution of above-mentioned silver nitrate and Two-dimensional Carbon compound, room temperature reaction 2h, after reaction terminates, is centrifuged gained suspension, gained precipitate with deionized water is washed three times, absolute ethanol washing three times, 80 DEG C of dry 12h of vacuum, obtain Two-dimensional Carbon compound (i.e. MXene) loaded Ag simple substance nano-powder, Product Labeling is A-1, Fig. 1 is its field emission scanning electron microscope photo, it can be seen that the Ag nano particle diameter of MXene area load is 20-400nm；Fig. 2 is its X ray diffracting spectrum, it will be apparent that occur in that the diffraction maximum of Ag simple substance.
Embodiment 2:
The preparation method of a kind of Two-dimensional Carbon compound carried metal simple substance Au nano-powder, comprises the steps:
(1) by 5g MAX phase Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M being dissolved with 5g lithium fluoride, magnetic agitation 48h at a temperature of 40 DEG C, centrifugation precipitates, clean to using washes of absolute alcohol again three times close to neutrality through deionized water, be vacuum dried 12h gained pressed powder at a temperature of 80 DEG C will be deposited in and be Two-dimensional Carbon compound；
(2) chlorauric acid solution measuring 10mL 0.01g/mL is dispersed in 50 mL deionized waters, and room temperature stirs evenly；It is dispersed in above-mentioned aqueous solution of chloraurate make blend solution by 0.5g Two-dimensional Carbon compound pressed powder, stirs；
(3) with vigorous stirring by the NaBH of 50mL 0.1mol/L4Aqueous solution is slowly added in the blend solution of above-mentioned gold chloride and Two-dimensional Carbon compound, room temperature reaction 2h, after reaction terminates, is centrifuged suspension, gained precipitate with deionized water is washed three times, absolute ethanol washing three times, 80 DEG C of dry 12h of vacuum, obtain Two-dimensional Carbon compound (i.e. MXene) load Au simple substance nano-powder, Product Labeling is A-2, Fig. 3 is its field emission scanning electron microscope photo, it can be seen that the Au nano particle diameter of MXene area load is 20-200nm；Fig. 4 is its X ray diffracting spectrum, it will be apparent that occur in that the diffraction maximum of Au simple substance.
Embodiment 3:
The preparation method of a kind of Two-dimensional Carbon compound carried metal simple substance Pd nano-powder, comprises the steps:
(1) by 5g MAX phase Ti3AlC2Powder is immersed in the hydrochloric acid solution of the 100mL 6M being dissolved with 5g lithium fluoride, magnetic agitation 48h at a temperature of 40 DEG C, centrifugation precipitates, clean to using washes of absolute alcohol again three times close to neutrality through deionized water, be vacuum dried 12h gained pressed powder at a temperature of 80 DEG C will be deposited in and be Two-dimensional Carbon compound；
(2) palladium chloride solution measuring 10mL 0.01g/mL is dispersed in 50 mL deionized waters, and room temperature stirs evenly；It is dispersed in above-mentioned palladium chloride aqueous solution make blend solution by 0.5g Two-dimensional Carbon compound pressed powder, stirs；
(3) with vigorous stirring by the NaBH of 50mL 0.1mol/L4Aqueous solution is slowly added in the blend solution of above-mentioned Palladous chloride. and Two-dimensional Carbon compound, room temperature reaction 2h, after reaction terminates, is centrifuged suspension, gained precipitate with deionized water is washed three times, absolute ethanol washing three times, 80 DEG C of dry 12h of vacuum, obtain Two-dimensional Carbon compound (i.e. MXene) load P d simple substance nano-powder, Product Labeling is A-3, Fig. 5 is its field emission scanning electron microscope photo, it can be seen that the Pd nano particle diameter of MXene area load is 10-200nm；Fig. 6 is its X ray diffracting spectrum, it will be apparent that occur in that the diffraction maximum of Pd simple substance.
The application in terms of photocatalytically degradating organic dye of the Two-dimensional Carbon compound carried metal simple substance nano-powder:
Methylene blue (MB) solution of preparation 10mg/L, take the Two-dimensional Carbon compound prepared by 100mg, embodiment 1 to 3 Two-dimensional Carbon compound (i.e. MXene) carried metal simple substance nano-powder respectively, it is dispersed in respectively in 100mL MB solution, under the conditions of lucifuge, magnetic agitation 30min is allowed to equilibrium adsorption, then solution is placed under photocatalysis apparatus and reacts, sample centrifugal segregation catalyst every 5min, use ultraviolet-uisible spectrophotometer to test subsequently.Test result is as shown in Figure 7, MXene loaded Ag nanoparticle can make methylene blue degraded more than 90% as photocatalyst after ultraviolet lighting 15min, load Au and Pd for 80% and 60%, i.e. photocatalytic after MXene has loaded metal simple-substance nanoparticle substantially has higher photocatalysis efficiency than pure MXene.
Finally, it is noted that the foregoing is only the preferred embodiment of the present invention, being not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement retouching etc. done, should be included within the scope of the present invention.
Claims (6)
1. the preparation method of a Two-dimensional Carbon compound carried metal simple substance nano-powder, it is characterised in that comprise the steps:
(1) being immersed in the hydrochloric acid solution being dissolved with lithium fluoride by MAX phase ceramics powder, stirring, centrifugation, successively with deionized water and ethanol purge, dried gained pressed powder is Two-dimensional Carbon compound；
(2) Two-dimensional Carbon compound being dissolved in aqueous metal salt and make blend solution, Two-dimensional Carbon compound concentration in blend solution is 8 ~ 10g/L；
(3) under stirring, reducing agent aqueous solution is joined in above-mentioned blend solution, reducing agent aqueous solution is 1 (1-1.2) with the volume ratio of blend solution, room temperature reaction 0.5-2h, after reaction terminates, being centrifuged by gained suspension, gained solid precipitation washs, is drying to obtain Two-dimensional Carbon compound carried metal simple substance nano-powder.
The preparation method of Two-dimensional Carbon compound carried metal simple substance nano-powder the most according to claim 1, it is characterised in that described Two-dimensional Carbon compound is Ti3C2、Ti2C or V2C。
The preparation method of Two-dimensional Carbon compound carried metal simple substance nano-powder the most according to claim 1, it is characterized in that, slaine in aqueous metal salt is at least one in silver nitrate, gold chloride, chloroplatinic acid, Palladous chloride., Palladous nitrate., radium chloride, rhodium nitrate, ruthenic chloride, nitric acid ruthenium, iron chloride, ferric nitrate, iron sulfate, cobaltous chloride, cobalt nitrate, cobalt acetate, cobaltous sulfate, Nickel dichloride., nickel nitrate, nickel sulfate, nickel acetate, copper chloride, copper nitrate, copper sulfate and copper acetate, and the concentration of aqueous metal salt is 0.01-0.1mol/L.
The preparation method of Two-dimensional Carbon compound carried metal simple substance nano-powder the most according to claim 1, it is characterised in that the reducing agent in reducing agent aqueous solution is NaBH4、KBH4、LiBH4, one or more combination in hydrazine hydrate and sodium citrate, wherein the concentration of reducing agent aqueous solution is 0.05-0.1mol/L.
5. use the arbitrary described Two-dimensional Carbon compound carried metal simple substance nano-powder obtained by preparation method of Claims 1-4.
6. the Two-dimensional Carbon compound carried metal simple substance nano-powder described in claim 5 is as photocatalyst application in terms of photocatalytic degradation dirt organic pollutants.
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