CN111330610A - Silver nanoflower/Ti3C2TxPreparation method and application of composite material - Google Patents
Silver nanoflower/Ti3C2TxPreparation method and application of composite material Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 43
- 239000004332 silver Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 239000002057 nanoflower Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 18
- 229910009819 Ti3C2 Inorganic materials 0.000 claims abstract description 36
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 9
- 230000009286 beneficial effect Effects 0.000 claims abstract description 4
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 4
- 241000446313 Lamella Species 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims abstract description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 42
- 239000007864 aqueous solution Substances 0.000 claims description 33
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 32
- 239000000243 solution Substances 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 18
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 16
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 15
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 15
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000002135 nanosheet Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 7
- 239000011941 photocatalyst Substances 0.000 claims description 6
- 230000000593 degrading effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 231100000614 poison Toxicity 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000003440 toxic substance Substances 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001782 photodegradation Methods 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000013329 compounding Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
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- 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
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a silver nanometer flower/Ti3C2TxA process for preparing a composite material, in particular Ti3C2TxComposite material obtained by loading silver nanoflower particles on a sheet layer, wherein Ti with a two-dimensional structure3C2TxThe lamella provides a stable framework and a larger specific surface area, and is beneficial to the catalytic reaction; the silver nanometer flower is composed ofSelf-assembled to silver flakes of 400-600 nm size and 10-30 nm thickness, which are supported on Ti3C2TxThe surface of the sheet layer, which forms a close contact interface with the sheet layer, becomes the active site of the composite material. Silver nanoflower/Ti prepared by the method of the invention3C2TxThe composite material is an efficient and stable photocatalytic material, can effectively degrade the organic dye rhodamine B, and has the photodegradation efficiency as high as 91.3 percent.
Description
Technical Field
The invention relates to a preparation method of a nano composite material, in particular to silver nanoflower/Ti3C2TxA preparation method and application of the composite material.
Background
Human beings in the 21 st century face problems of environmental pollution, energy shortage and the like, and the photocatalysis technology is concerned about solving the problem of environmental pollution by converting cheap, clean and renewable solar energy into chemical energy and solving the problem of energy by degrading organic pollutants or hydrogen production by utilizing the chemical energy. Therefore, the research on photocatalytic materials has been increased in recent years. Among numerous photocatalytic materials, the composite structure of nano-silver/two-dimensional layered material becomes one of the research hotspots because the strong visible light response characteristic of nano-silver and the large specific surface area characteristic of two-dimensional layered material can be simultaneously utilized.
Some methods for preparing nano silver/two-dimensional layered material composite structures are reported at present. For example, CN201910684608.3 and CN201710105010.5 respectively adopt a photo-initiation method and a solvothermal method to prepare Ag/PANI/graphene and Ag/g-C3N4A composite photocatalyst is provided. Although the method successfully prepares the nano silver/two-dimensional layered material composite structure, some toxic substances are generated in the reaction process, and the preparation process is complex. The present invention reports a successful preparation of two-dimensional Ti3C2TxThe surface of the nano sheet is loaded with silver nano flower composite materialMethod in which Ti3C2TxIs a two-dimensional layered transition metal compound with a graphene-like structure, TxRepresents a functional group-OH, -F, etc. The method has the advantages of no toxicity, high efficiency, simple process and the like, and the composite material prepared by the method shows high-efficiency visible light degradation activity.
Disclosure of Invention
The invention provides a silver nanoflower/Ti composite photocatalyst aiming at the defect of complex preparation of a nano-silver/two-dimensional layered material composite photocatalyst3C2TxA preparation method and application of the composite material.
The silver nanoflower/Ti of the invention3C2TxThe preparation method of the composite material comprises the following steps:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Uniformly stirring the powder, heating the powder in water bath at 70 ℃ for 45 hours, and centrifugally washing the powder to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: utilizing the Ti prepared in step 13C2TxSol to realize the loading of the silver nanoflowers, and the specific steps are as follows: sequentially adding ammonium citrate aqueous solution and polyvinylpyrrolidone aqueous solution with certain concentration into the prepared silver nitrate aqueous solution, and uniformly stirring; followed by addition of Ti obtained in step 13C2TxDissolving the sol, and uniformly stirring again to obtain a mixed solution; heating the mixed solution in water bath at 25-70 ℃ for 2-45 hours, centrifuging and drying after the reaction is finished to obtain silver nanoflower/Ti3C2TxA composite material.
In step 1, lithium fluoride, hydrochloric acid and Ti3AlC2In a molar ratio of 8:24: 1.
In the step 2, the concentration of the ammonium citrate aqueous solution is 11.6-11.8 mg/mL, the concentration of the polyvinylpyrrolidone aqueous solution is 10.0-10.2 mg/mL, and the concentration of the silver nitrate aqueous solution is 10.0-10.2 mg/mL.
Further, silver nitrate solution, ammonium citrate aqueous solution, polyvinylpyrrolidone aqueous solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1.
The silver nanoflower/Ti of the invention3C2TxComposite material of Ti3C2TxThe composite material of silver nanoflower particles is loaded on the sheet layer. Wherein Ti of two-dimensional structure3C2TxThe lamella provides a stable framework and a larger specific surface area, and is beneficial to the catalytic reaction; the silver nanoflower is formed by self-assembling silver sheets with large transverse size (400-600 nm) and ultrathin thickness (10-30 nm), and the silver nanoflower is loaded on Ti3C2TxThe surface of the sheet layer, which forms a close contact interface with the sheet layer, becomes the active site of the composite material.
The silver nanoflower/Ti of the invention3C2TxThe composite material can be used as an efficient and stable photocatalyst for degrading toxic substances, and the degradation of harmful dye rhodamine-B is taken as an example: at room temperature, a 250W xenon light cold light lamp is used for carrying out irradiation degradation on rhodamine-B aqueous solution (the concentration is 0.0075g/L) simulated into a natural sewage environment, and then a fluorescence spectrophotometer is used for analyzing the rhodamine-B aqueous solution in silver nanoflower/Ti3C2TxDegradation degree of rhodamine-B under action of composite material (every 30mL of solution is added with 25mg of silver nanoflower/Ti3C2TxComposite materials). Under the simulated natural condition of a xenon cold light lamp, the degradation rate of rhodamine-B can reach 91.3 percent within 3 hours.
The invention has the beneficial effects that:
(1) the invention uses a simple one-step reduction method to prepare two-dimensional Ti3C2TxThe nano-sheet is compounded with the silver nanoflower with strong visible light response, and the preparation method is simple and non-toxic;
(2) the silver nanoflower and the two-dimensional Ti provided by the invention3C2TxThe conditions in the compounding process are mild, the compounding process is quick and easy to obtain, and the silver nanoflower/Ti generated after the reaction is finished3C2TxThe composite material is higher than the previous researchThe specific surface area of the catalyst can provide more active sites to promote the catalytic reaction;
(3) the silver nanometer flower/Ti prepared by the method3C2TxThe nano composite structure can inhibit the generation of electron-hole pairs, thereby showing excellent capacity of degrading rhodamine-B under visible light and having great application prospect in the field of photocatalysis.
Drawings
FIG. 1 shows silver nanoflower/Ti prepared in example 23C2TxX-ray diffraction spectra of the composite.
FIG. 2 shows silver nanoflower/Ti prepared in example 33C2TxScanning electron micrographs of the composite.
FIG. 3 shows silver nanoflower/Ti prepared in example 43C2TxThe effect diagram of the composite material as a photocatalyst for degrading rhodamine B is shown.
Detailed Description
Example 1:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Powder of lithium fluoride, hydrochloric acid and Ti3AlC2Is in a molar ratio of 8:24:1, stirring for 5min, heating in water bath at 70 ℃ for 45h, and centrifuging and washing to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: adding 11.6mg/mL ammonium citrate aqueous solution and 10.0mg/mL polyvinylpyrrolidone aqueous solution into 3.8mg/mL silver nitrate aqueous solution prepared in advance, and stirring for 5 min; then, taking the Ti obtained in the step 1 by using a rubber head dropper3C2TxAdding the sol into the liquid, and stirring for 5min to obtain mixed solution containing silver nitrate solution, ammonium citrate solution, polyvinylpyrrolidone solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1; heating the mixed solution in water bath at 70 deg.C for 2 hr, and taking out the mixed solutionCentrifuging and washing with a centrifuge at 9000r/min for three times, centrifuging for 5min each time, and drying the washed product in a vacuum drying oven at 70 deg.C for 24 hr to obtain silver nanoflower/Ti powder3C2TxA composite material.
Example 2:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Powder of lithium fluoride, hydrochloric acid and Ti3AlC2Is in a molar ratio of 8:24:1, stirring for 5min, heating in water bath at 70 ℃ for 45h, and centrifuging and washing to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: adding 11.6mg/mL ammonium citrate aqueous solution and 10.0mg/mL polyvinylpyrrolidone aqueous solution into 3.8mg/mL silver nitrate aqueous solution prepared in advance, and stirring for 5 min; then, taking the Ti obtained in the step 1 by using a rubber head dropper3C2TxAdding the sol into the liquid, and stirring for 5min to obtain mixed solution containing silver nitrate solution, ammonium citrate solution, polyvinylpyrrolidone solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1; heating the mixed solution in water bath at 70 deg.C for 24 hr, taking out the mixed solution, centrifuging and washing with centrifuge at 9000r/min for three times, each time for 5min, and drying the washed product in vacuum drying oven at 70 deg.C for 24 hr to obtain silver nanoflower/Ti3C2TxA composite material.
Example 3:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Powder of lithium fluoride, hydrochloric acid and Ti3AlC2Is in a molar ratio of 8:24:1, stirring for 5min, heating in water bath at 70 ℃ for 45h, and centrifuging and washing to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: adding 11.8mg/mL ammonium citrate aqueous solution and 10.2mg/mL polyvinylpyrrolidone aqueous solution into 4.0mg/mL silver nitrate aqueous solution prepared in advance, stirring for 5min, and then taking the Ti obtained in the step 1 by using a rubber head dropper3C2TxAdding the sol into the liquid, and stirring for 5min to obtain mixed solution containing silver nitrate solution, ammonium citrate solution, polyvinylpyrrolidone solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1; heating the mixed solution in water bath at 25 deg.C for 18 hr, taking out the mixed solution, centrifuging and washing with centrifuge at 9000r/min for three times, each time for 5min, and drying the washed product in vacuum drying oven at 70 deg.C for 24 hr to obtain silver nanoflower/Ti3C2TxA composite material.
Example 4:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Powder of lithium fluoride, hydrochloric acid and Ti3AlC2Is in a molar ratio of 8:24:1, stirring for 5min, heating in water bath at 70 ℃ for 45h, and centrifuging and washing to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: adding 11.6mg/mL ammonium citrate aqueous solution and 10.0mg/mL polyvinylpyrrolidone aqueous solution into 3.8mg/mL silver nitrate aqueous solution prepared in advance, stirring for 5min, and then taking the Ti obtained in the step 1 by using a rubber head dropper3C2TxAdding the sol into the liquid, and stirring for 5min to obtain mixed solution containing silver nitrate solution, ammonium citrate solution, polyvinylpyrrolidone solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1; heating the mixed solution in 70 deg.C water bath for 45 hr, taking out the mixed solution, centrifuging and washing with centrifuge at 9000r/min for three times, each time for 5min, and drying the washed product in 70 deg.C vacuum drying oven for 24 hr to obtain silver nanoflower/Ti3C2TxA composite material.
Example 5:
step 1: firstly, adding lithium fluoride into a hydrochloric acid (6M) solution to prepare a lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Powder of lithium fluoride, hydrochloric acid and Ti3AlC2Is in a molar ratio of 8:24:1, stirring for 5min, heating in water bath at 70 ℃ for 45h, and centrifuging and washing to obtain two-dimensional Ti3C2TxAnd dispersing the nano-sheets in deionized water to prepare sol, and sealing and storing for later use.
Step 2: adding 11.6mg/mL ammonium citrate aqueous solution and 10.0mg/mL polyvinylpyrrolidone aqueous solution into 3.8mg/mL silver nitrate aqueous solution prepared in advance, stirring for 5min, and then taking the Ti obtained in the step 1 by using a rubber head dropper3C2TxAdding the sol into the liquid, and stirring for 5min to obtain mixed solution containing silver nitrate solution, ammonium citrate solution, polyvinylpyrrolidone solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1; heating the mixed solution in water bath at 25 deg.C for 45 hr, taking out the mixed solution, centrifuging and washing with centrifuge at 9000r/min for three times, each time for 5min, and drying the washed product in vacuum drying oven at 70 deg.C for 24 hr to obtain silver nanoflower/Ti3C2TxA composite material.
Claims (6)
1. Silver nanoflower/Ti3C2TxThe preparation method of the composite material is characterized by comprising the following steps:
the silver nanoflower/Ti3C2TxComposite material of Ti3C2TxComposite material obtained by loading silver nanoflower particles on a sheet layer, wherein Ti with a two-dimensional structure3C2TxThe lamella provides a stable framework and a larger specific surface area, and is beneficial to the catalytic reaction; the silver nanoflower is formed by self-assembling silver sheets with the transverse size of 400-600 nm and the thickness of 10-30 nm, and the silver nanoflower is loaded on Ti3C2TxThe surface of the sheet, formed closely with itBecomes an active site of the composite material.
2. The method of claim 1, comprising the steps of:
step 1: firstly, adding lithium fluoride into hydrochloric acid solution to prepare lithium fluoride acid solution with the concentration of 50mg/mL, and then adding a certain amount of Ti3AlC2Uniformly stirring the powder, heating the powder in water bath at 70 ℃ for 45 hours, and centrifugally washing the powder to obtain two-dimensional Ti3C2TxNano sheets, dispersing the nano sheets in deionized water to prepare sol, and sealing and storing the sol for later use;
step 2: utilizing the Ti prepared in step 13C2TxSol to realize the loading of the silver nanoflowers, and the specific steps are as follows: sequentially adding ammonium citrate aqueous solution and polyvinylpyrrolidone aqueous solution with certain concentration into the prepared silver nitrate aqueous solution, and uniformly stirring; followed by addition of Ti obtained in step 13C2TxDissolving the sol, and uniformly stirring again to obtain a mixed solution; heating the mixed solution in water bath at 25-70 ℃ for 2-45 hours, centrifuging and drying after the reaction is finished to obtain silver nanoflower/Ti3C2TxA composite material.
3. The method of claim 2, wherein:
in step 1, lithium fluoride, hydrochloric acid and Ti3AlC2In a molar ratio of 8:24: 1.
4. The method of claim 2, wherein:
in the step 2, the concentration of the ammonium citrate aqueous solution is 11.6-11.8 mg/mL, the concentration of the polyvinylpyrrolidone aqueous solution is 10.0-10.2 mg/mL, and the concentration of the silver nitrate aqueous solution is 10.0-10.2 mg/mL.
5. The method of claim 4, wherein:
silver nitrate solution, ammonium citrate aqueous solution and polyvinyl pyridinePyrrolidone aqueous solution and Ti3C2TxThe volume ratio of the sol is 6:6:6: 1.
6. Silver nanoflower/Ti obtained by any one of the preparation methods according to claims 1 to 53C2TxThe application of the composite material is characterized in that:
the silver nanoflower/Ti3C2TxThe composite material is used as a photocatalyst in the process of degrading toxic substances, wherein the toxic substances comprise a harmful dye rhodamine-B and the like.
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| CN113559899A (en) * | 2021-07-08 | 2021-10-29 | 西南科技大学 | Silver-loaded multilayer Ti for uranium reduction separation3C2TxPreparation and application of MXene |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100150801A1 (en) * | 2007-09-19 | 2010-06-17 | General Electric Company | FORMED CATALYST FOR NOx REDUCTION |
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN106459550A (en) * | 2014-06-23 | 2017-02-22 | 出光兴产株式会社 | Thermosetting composition and method for producing thermosetting resin |
| CN106622318A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Layered composite photocatalyst using bimetallic nanoparticles as heterojunctions and preparation method thereof |
| CN108213771A (en) * | 2018-01-15 | 2018-06-29 | 合肥工业大学 | A kind of composite soldering and its soldering processes for soldering silicon carbide ceramics in vacuum |
| CN109012663A (en) * | 2018-07-27 | 2018-12-18 | 范唯凌 | A kind of nano silver/carbon composite photocatalyst material and its preparation method and application |
| CN109827945A (en) * | 2019-02-28 | 2019-05-31 | 合肥工业大学 | A kind of preparation method of high SERS activity Ag/MXene-Ti3C2 composite material |
| CN110508313A (en) * | 2019-09-05 | 2019-11-29 | 安徽工业大学 | With the method for Ag-Pd nanometer sheet catalyst visible light catalytic formate dehydrogenase |
-
2020
- 2020-04-10 CN CN202010277381.3A patent/CN111330610A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100150801A1 (en) * | 2007-09-19 | 2010-06-17 | General Electric Company | FORMED CATALYST FOR NOx REDUCTION |
| CN106459550A (en) * | 2014-06-23 | 2017-02-22 | 出光兴产株式会社 | Thermosetting composition and method for producing thermosetting resin |
| CN105854913A (en) * | 2016-04-07 | 2016-08-17 | 河南理工大学 | Two-dimension carbide loaded metal simple substance nano-powder, and preparation method and application thereof |
| CN106622318A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Layered composite photocatalyst using bimetallic nanoparticles as heterojunctions and preparation method thereof |
| CN108213771A (en) * | 2018-01-15 | 2018-06-29 | 合肥工业大学 | A kind of composite soldering and its soldering processes for soldering silicon carbide ceramics in vacuum |
| CN109012663A (en) * | 2018-07-27 | 2018-12-18 | 范唯凌 | A kind of nano silver/carbon composite photocatalyst material and its preparation method and application |
| CN109827945A (en) * | 2019-02-28 | 2019-05-31 | 合肥工业大学 | A kind of preparation method of high SERS activity Ag/MXene-Ti3C2 composite material |
| CN110508313A (en) * | 2019-09-05 | 2019-11-29 | 安徽工业大学 | With the method for Ag-Pd nanometer sheet catalyst visible light catalytic formate dehydrogenase |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113559899A (en) * | 2021-07-08 | 2021-10-29 | 西南科技大学 | Silver-loaded multilayer Ti for uranium reduction separation3C2TxPreparation and application of MXene |
| CN113559899B (en) * | 2021-07-08 | 2023-11-24 | 西南科技大学 | Uranium reduction separated silver-loaded multilayer Ti 3 C 2 T x Preparation and application of MXene |
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