CN105948120B - A kind of vanadic anhydride micro-nano particle and its preparation method and application - Google Patents
A kind of vanadic anhydride micro-nano particle and its preparation method and application Download PDFInfo
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- CN105948120B CN105948120B CN201610269565.9A CN201610269565A CN105948120B CN 105948120 B CN105948120 B CN 105948120B CN 201610269565 A CN201610269565 A CN 201610269565A CN 105948120 B CN105948120 B CN 105948120B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention provides a kind of micro-nano particle, the micro-nano particle is vanadic anhydride micro-nano particle, is self-assembly of by nanometer sheet.Present invention also offers the preparation method of the micro-nano particle, it the described method comprises the following steps and 1) add vanadic anhydride in ethylene glycol, stirring is well mixed it, forms suspending liquid A；2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；3) heat suspension B, after be stored at room temperature cooling, obtain the predecessor containing black precipitate；4) by step 3) mixed solution containing the predecessor that is formed centrifuges, washs and dry, obtain the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of；5) by step 4) obtained predecessor calcines in air atmosphere, obtains the micro-nano particle.Present invention also offers the micro-nano particle new energy, environment measuring, food and medical domain application.
Description
Technical field
The present invention relates to field of nanometer technology, in particular to a kind of micro-nano particle and its preparation method and application.
Background technology
Vanadium oxide nano particle is due to its unique lamellar structure, the property such as outstanding light, electricity, magnetic, in lithium battery, gas
Sensing and catalytic field have very outstanding performance, receive the extensive concern of people.Vanadium oxide mainly includes three kinds of oxygen
Compound：Vanadic anhydride, vanadium dioxide and vanadium trioxide.Different vanadium oxides are according to property different application in different fields.
This patent is only sketched due to relating only to vanadic anhydride to it.Vanadic anhydride is used as traditional production sulfuric acid
Catalyst be known.In this year, as the research to its nanostructured is gradually goed deep into, it is gentle in lithium ion battery
The premium properties produced in terms of body sensing is by people's extensive concern.According to the literature, its vanadium pentoxide nanowires is to n-butylamine
It is very sensitive, response can be produced to the n-butylamine of thousand a ten thousandth concentration.This will play important in food and biological life science
Effect.
It is well known that the property and application performance of nano material are heavily dependent on its granule-morphology and size.And
Granule-morphology and size often have close contact with synthetic method and path.The flower-shaped micro-nano that nanometer sheet is self-assembly of
Grain, because it has three-dimensional structure, using the teaching of the invention it is possible to provide the more adsorption potentials of gas, has in gas sensing and gas phase catalysis field
Outstanding performance.On the flower-shaped micro-nano particle of nanometer sheet self assembly, there are some reports at present.Method is concentrated mainly on two
Kind：(1) vanadyl acetylacetonate is dissolved in 20 milliliters of ethanol, 30 milliliters of hydrogen peroxide is added afterwards.Liquid mixed above is placed on 150
Heated 24 hours in DEG C autoclave.Calcined 2 hours under 400 DEG C of air after the separation of obtained precipitation is dried, the shape can be obtained
Looks vanadium oxide particles.(2) ammonium metavanadate is dissolved in 50 ml deionized waters, system pH is adjusted to 2 using nitric acid, and
The stirring at 50 DEG C is until there is orange precipitation.20 ml methanols are added into above solution, 24 hours are stood at room temperature.Precipitation becomes
Washing is isolated during into darkorange.Darkorange precipitation is the vanadium oxide particles of floriform appearance.Other method
The pattern of synthesis has obvious difference, such as sea urchin shape vanadic anhydride micron particles, Yi Jihua with above-mentioned vanadium oxide particles
The vanadium pentoxide films of shape pattern.
Above method cost of material is higher, and method is complicated, and product has spent acid generation, and inadequate environmental protection is not suitable for big rule
Mould is produced, and huge inconvenience is brought to follow-up use.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of micro-nano particle, and the micro-nano particle has lamella nanostructured simultaneously
With flower-shaped spherical micrometer structure.
The second object of the present invention is to provide a kind of preparation method of the micro-nano particle, this method is simple to operate, into
This cheap, safety and environmental protection, can be with large-scale application in actual production.
The third object of the present invention is the application for providing the micro-nano particle, and the micro-nano particle has a wide range of application
It is general, it is adaptable in new energy, environment measuring and food and medical domain.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
One aspect of the present invention is related to a kind of micro-nano particle, and the micro-nano particle is vanadic anhydride micro-nano particle, by
Nanometer sheet is self-assembly of.
The micro-nano particle formed is assembled by nanometer sheet has micron-sized macro-size, meanwhile, its surface area ratio is common
Micro-nano particle is much larger, therefore its adsorption area is very big.
Preferably, the micro-nano particle is flower-shaped micro-nano particle.
Flower-shaped micro-nano particle has good gas sensing performance, and obvious resistance reduction is had after its adsorbed gas.
Another aspect of the present invention is related to the preparation method of described micro-nano particle, the described method comprises the following steps：
1) vanadic anhydride is added in ethylene glycol, stirring is well mixed it, forms suspending liquid A；
2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；
Adding sodium carbonate liquor can promote in subsequent reactions, and the oxyvanadium compound of sheet is flower-shaped by being self-assembly of
Micro-nano particle.
3) heat suspension B, after be stored at room temperature cooling, obtain the predecessor containing black precipitate；
Heat suspension so that vanadic anhydride is dissolved in ethylene glycol, and chemically reacts therewith, generate sheet output.
4) by step 3) mixed solution containing the presoma that is formed centrifuges, washs and dry, received
The flower-shaped vanadium oxide predecessor that rice piece is self-assembly of；
5) by step 4) obtained predecessor calcines in air atmosphere, obtains the micro-nano particle.
Calcine in atmosphere so that predecessor by the oxygen complete oxidation in air, is formed pure five oxidation at high temperature
The micro-nano particle that two vanadium are constituted.
In the method for the present invention, the used equal safety and environmental protection of reagent, and source is easy to get with low cost, the present invention is used
Method mild condition.
Preferably, the step 1) in stirring carried out in 50-70 DEG C of water-bath, five oxygen described in the suspending liquid A
It is 0.075-0.3mM to change two vanadium relative to the molar concentration of ethylene glycol.
The excessive concentration of vanadic anhydride can cause the micro-nano particle formed in subsequent reactions excessive, and its concentration it is too low when
Then it can lead to not to form particle.
Preferably, the molar concentration of the sodium bicarbonate solution is 1-1.5M.
Preferably, the step 2) in sodium bicarbonate solution addition be 1-10mL.
Sodium acid carbonate concentration is 1-1.5M, when addition is 1-10ml, and the ability that it promotes micro-nano particle to generate is most strong.
Preferably, the step 3) in, the suspension B is heated to 180-260 DEG C, and the heat time is 12-36 hours.
Heating is preferably carried out under elevated pressure conditions, therefore suspension B can be heated to 180-260 DEG C, be added with the temperature
Hot suspension can cause vanadic anhydride to be dissolved in ethylene glycol, and concurrent biochemical reaction, the sheet of generation barium oxide is sunk
Form sediment.
Preferably, the step 4) in, washed using ethanol and deionized water, the drying is under conditions of 50-80 DEG C
Carry out.
Preferably, the temperature of the calcining is 400-600 DEG C, and calcination time is 2-6 hours.
The fusing point of vanadic anhydride is 690 DEG C, and the calcining heat of 400-600 DEG C of selection can cause presoma quilt completely
Vanadic anhydride is sintered into, while not destroying the flower-shaped configuration of surface of generated micro-nano particle.
Another aspect of the present invention is related to the micro-nano particle answering in new energy, environment measuring, food and medical domain
With.
Compared with prior art, beneficial effects of the present invention are：
(1) present invention synthesizes the forerunner for the flower-shaped micro-nano particle that nanoscale twins are self-assembly of in ethylene glycol solution first
Thing.
(2) the barium oxide micro-nano particle after being formed has very high specific surface area, and stronger structural stability.This meeting
Contribute to it as the raising of electricity material and the performance of gas sensing material.
(3) the flower-shaped barium oxide particle that nanometer sheet is self-assembly of is provided simultaneously with lamella nanostructured and flower-shaped spherical
Micrometer structure.Lamella nanostructured contributes to device figure layer to its leading role of application function, flower-shaped spherical micrometer structure
Assembling.
(4) preparation method for the flower-shaped micro-nano particle that nanometer sheet provided by the present invention is self-assembly of it is simple to operate, into
Sheet is cheap, possess the possibility largely produced, in new energy (lithium battery), environment measuring and food and medical domain (gas sensing
Device) have a wide range of applications.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the accompanying drawing used required in technology description to be briefly described.
Fig. 1 is preparation manipulation scheme sketch of the invention
Fig. 2 is the flower-shaped vanadium oxide micro-nano predecessor scanning that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
Electromicroscopic photograph.
Fig. 3 is the flower-shaped vanadic anhydride micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of.
Fig. 4 is the X-ray for the flower-shaped predecessor micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
Diffracting spectrum.
Fig. 5 is the X for the flower-shaped vanadic anhydride micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of
X ray diffraction collection of illustrative plates.
Fig. 6 is that the flower-shaped vanadic anhydride micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of is made
The relation of sensitiveness and tested gas concentration for gas sensing material.
Fig. 7 is that the flower-shaped vanadic anhydride micro-nano particle that the nanometer sheet prepared by the embodiment of the present invention 1 is self-assembly of is made
For the selectivity of gas sensing material.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted specific in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, be
The conventional products that can be obtained by commercially available purchase.
Embodiment 1
Micro-nano particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours, makes it in being bathed in 50 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.075mM；
1.2) 1mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.5M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 180 DEG C, and the heat time is 12 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, is dried at 50 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
2) preparation for the flower-shaped vanadic anhydride micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in air atmosphere
Shape vanadic anhydride micro-nano particle.Calcining heat is 400 DEG C, and calcination time is 6 hours.
Embodiment 2
Micro-nano particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours, makes it in being bathed in 70 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.3mM；
1.2) 10mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 260 DEG C, and the heat time is 36 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, is dried at 70 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
2) preparation for the flower-shaped vanadic anhydride micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in air atmosphere
Shape vanadic anhydride micro-nano particle.Calcining heat is 600 DEG C, and calcination time is 2 hours.
Embodiment 3
Micro-nano particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours, makes it in being bathed in 60 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.15mM；
1.2) 5mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.25M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 220 DEG C, and the heat time is 24 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, is dried at 60 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
2) preparation for the flower-shaped vanadic anhydride micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in air atmosphere
Shape vanadic anhydride micro-nano particle.Calcining heat is 600 DEG C, and calcination time is 4 hours.
Embodiment 4
Micro-nano particle is prepared according to following steps：
1) synthesis for the flower-shaped vanadium oxide predecessor that nanometer sheet is self-assembly of：
1.1) commercial vanadic anhydride is added in ethylene glycol solution, strong agitation 2 hours, makes it in being bathed in 60 DEG C of water
It is well mixed, form suspending liquid A；The molar concentration of the suspending liquid A is 0.2mM；
1.2) 7mL sodium bicarbonate solutions are added into suspending liquid A, the color of suspension is changed into light yellow from brown color,
Suspension B is formed, wherein, the molar concentration of the sodium bicarbonate solution is 1.3M；
1.3) suspension B is put into autoclave and heated, heating-up temperature is 200 DEG C, and the heat time is 24 hours, and room temperature is quiet
The predecessor containing black precipitate can be arrived after putting cooling；
1.4) by step 1.3) formed containing precipitation product mixed solution centrifuge, centrifugal rotational speed is 2000-
3000rpm, is washed with ethanol and deionized water, is dried at 60 DEG C.Obtain before the flower-shaped vanadium oxide that nanometer sheet is self-assembly of
Drive thing.
2) preparation for the flower-shaped vanadic anhydride micro-nano particle that nanometer sheet is self-assembly of：
2.1) by step 1.4) obtained predecessor calcines can obtain the flower that nanometer sheet is self-assembly of in air atmosphere
Shape vanadic anhydride micro-nano particle.Calcining heat is 500 DEG C, and calcination time is 4 hours.
Experimental example
Utilize vanadic anhydride flower-shaped micro-nano of the commercial gas sensing testing instrument (WS-30A, Henan, bright Sheng) to synthesis
Particle and sea urchin shape micro-nano particle carry out comparative gas sensing test.Wherein " respond " and be defined as：The aerial material of exposure
Expect the ratio of resistance (Ra) and the material resistance (Rg) in object gas.Fig. 6 shows the material of two kinds of structures in work
To the sensed events of the butylamine of various concentrations (5-200ppm) 1 when temperature is 300 DEG C.The bright flower-shaped micro-nano particle of the chart is in 5-
Higher response is respectively provided with compared to sea urchin shape micro-nano particle under 200ppm concentration, especially in high concentration (50-200ppm), it rings
2 times of sea urchin shape micro-nano particle should be almost, shows the face perception with the outstanding butylamine of detection 1.Fig. 7 shows two kinds of structural woods
Expect the selectivity for 100ppm VOC gas at 300 DEG C to various concentrations.The property shows that gas is passed
Sense material detects the ability of certain gas in mixed gas.Fig. 7 shows compared with acetone, ethanol, methanol and butanol, the gas
Body sensing material has very strong detectivity in terms of 1 butylamine is detected.Equally, compared to sea urchin shape micro-nano particle, the flower of this patent
1 butylamine of shape nano particle is selectively stronger.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (8)
1. a kind of preparation method of vanadic anhydride micro-nano particle, it is characterised in that the described method comprises the following steps：
1) vanadic anhydride is added in ethylene glycol, stirring is well mixed it, forms suspending liquid A；
2) sodium bicarbonate solution is added to suspending liquid A, forms suspension B；
3) hydro-thermal method heating suspension B, after be stored at room temperature cooling, obtain the predecessor containing black precipitate；
4) by step 3) mixed solution containing the predecessor that is formed centrifuges, washs and dry, obtain nanometer sheet
The flower-shaped vanadium oxide predecessor being self-assembly of；
5) by step 4) obtained predecessor calcines in air atmosphere, obtains the micro-nano particle；
The micro-nano particle is the flower-shaped particle that flake nano structure is self-assembly of, and the particle diameter of the micro-nano particle is micro- for 4-5
Rice, specific surface area is 61.5 square metres every gram.
2. according to the method described in claim 1, it is characterised in that the lamellar structure of flower-shaped particle is constituted in the micro-nano particle
Thickness is 10 nanometers, and purity is 99.5%, and essential element is 5 valency vanadium and divalent oxygen element.
3. the stirring according to the method described in claim 1, it is characterised in that the step 1) is in 50-70 DEG C of water-bath
Carry out, vanadic anhydride described in the suspending liquid A is 0.075-0.3mM relative to the molar concentration of ethylene glycol.
4. according to the method described in claim 1, it is characterised in that the molar concentration of the sodium bicarbonate solution is 1-1.5M.
5. the addition of sodium bicarbonate solution is 1- according to the method described in claim 1, it is characterised in that the step 2)
10mL/16mL suspending liquid As.
6. according to the method described in claim 1, it is characterised in that the step 3), the suspension B is heated to 180-
260 DEG C, the heat time is 12-36 hours.
7. according to the method described in claim 1, it is characterised in that the step 4), washed using ethanol and deionized water,
The drying is carried out under conditions of 50-80 DEG C.
8. according to the method described in claim 1, it is characterised in that the temperature of the calcining is 400-600 DEG C, calcination time is
2-6 hours.
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| CN107086132B (en) * | 2017-04-26 | 2019-07-19 | 安徽师范大学 | Flower-shaped three nickel nano film of vanadic anhydride/curing and its preparation method and application |
| CN107102036B (en) * | 2017-06-02 | 2019-10-01 | 东北大学 | The preparation method of the vanadium oxide particles of gold load |
| CN108847483A (en) * | 2018-06-21 | 2018-11-20 | 北京理工大学 | A kind of quick magnanimity preparation V2O5The method and application of nanometer sheet |
| CN109205674B (en) * | 2018-11-19 | 2020-04-07 | 北京科技大学 | Method for preparing vanadium pentoxide-based nanosheets |
| CN114288942A (en) * | 2021-11-18 | 2022-04-08 | 攀钢集团研究院有限公司 | Preparation method of spherical vanadium pentoxide particles |
| CN114212819B (en) * | 2021-12-16 | 2023-06-30 | 福州大学 | Radial vanadium pentoxide and application thereof to capacitor electrode |
| CN115663169B (en) * | 2022-12-13 | 2023-03-21 | 北京科技大学 | Vanadium oxide nanoflower and preparation method thereof |
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