CN113578351A - Pyrite iron disulfide/titanium dioxide composite material and preparation method and application thereof - Google Patents
Pyrite iron disulfide/titanium dioxide composite material and preparation method and application thereof Download PDFInfo
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- CN113578351A CN113578351A CN202110885706.0A CN202110885706A CN113578351A CN 113578351 A CN113578351 A CN 113578351A CN 202110885706 A CN202110885706 A CN 202110885706A CN 113578351 A CN113578351 A CN 113578351A
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- titanium dioxide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 229910052683 pyrite Inorganic materials 0.000 title claims abstract description 82
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 48
- 239000011028 pyrite Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- NFMAZVUSKIJEIH-UHFFFAOYSA-N bis(sulfanylidene)iron Chemical compound S=[Fe]=S NFMAZVUSKIJEIH-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910000339 iron disulfide Inorganic materials 0.000 title claims abstract description 33
- 229910052960 marcasite Inorganic materials 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 44
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002245 particle Substances 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims description 41
- 238000000034 method Methods 0.000 claims description 33
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 21
- 238000001238 wet grinding Methods 0.000 claims description 20
- 239000002105 nanoparticle Substances 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 9
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000010405 anode material Substances 0.000 claims description 4
- 239000003344 environmental pollutant Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 231100000719 pollutant Toxicity 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000007774 positive electrode material Substances 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 2
- 230000003115 biocidal effect Effects 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 239000002086 nanomaterial Substances 0.000 abstract description 5
- 230000001681 protective effect Effects 0.000 abstract description 5
- 238000009826 distribution Methods 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 7
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229940095991 ferrous disulfide Drugs 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere 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
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
- A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
- A61L2/08—Radiation
- A61L2/088—Radiation using a photocatalyst or photosensitiser
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
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- B82—NANOTECHNOLOGY
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention relates to the technical field of functional material preparation, and aims to solve the problem of FeS in the prior art2/TiO2The invention provides a pyrite iron disulfide/titanium dioxide composite material and a preparation method and application thereof, and aims to solve the problems of complex preparation process, low yield, large size, agglomeration and uneven component distribution of the composite material2/TiO2The preparation method of the nano material is simple, protective gas does not need to be added in the reaction process, the problem of secondary pollution does not exist in the middle, the yield is high, and the TiO is2Further reduces FeS2The size of the particles. In addition, the prepared FeS2/TiO2The composite material is not combined in a pure physical sense, and Fe and S are doped into TiO2In the lattice structure, the material performance is further improved.
Description
Technical Field
The invention relates to the technical field of functional material preparation, in particular to a pyrite iron disulfide/titanium dioxide composite material and a preparation method and application thereof.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the development of modern technology, the human resource consumption degree is getting larger and larger, the contradiction with nature is continuously excited, and the energy and environment problems become important problems to be solved urgently. Ferrous disulfide is a nontoxic environment-friendly indirect band gap semiconductor material with abundant reserves in the nature, and the band gap width is 0.95 eV. Very close to the requirement of 1.1eV required by an ideal solar cell material and simultaneously has the advantages ofHas excellent light absorption capacity and absorption coefficient up to 105cm-1. Ferrous disulfide material is therefore a new photovoltaic material with great potential.
FeS2The material has proper forbidden band width and higher light absorption coefficient, can be used for manufacturing extremely thin (less than 200nm) solar thin-film batteries, has the advantages of low price, rich resources, no toxicity and good environmental compatibility, is suitable for large-scale production, and is considered as a solar electrode material with great development potential. But natural FeS2Due to the problems of high impurity content, large particle size and the like, the actual electrochemical performance of the product is far from the theoretical value, and further treatment is needed to improve the discharge performance of the product.
FeS2/TiO2The excellent characteristics of the composite material enable the composite material to be applied to lithium ion battery anode materials, photocatalytic degradation pollutants, solar battery materials, photocatalytic water splitting hydrogen production, antibiosis and photocatalytic reduction of CO2Has wide application prospect in the fields of preparing methanol and the like.
Currently existing preparation of FeS2/TiO2The method of the composite material mainly comprises the following steps: hydrothermal method, solvent chemical reaction method, sol-gel-sulfurization method, magnetron sputtering-sulfurization method, electrostatic spinning method, direct mixing method, etc. The inventors found that in most of hydrothermal methods, solvent chemical reaction methods and the like, FeS is produced by chemically reacting iron ions with a sulfur source in a liquid phase system2The method has the defects of complex preparation process, easy secondary pollution, limited product yield and the like; the sol-gel-vulcanization method, the magnetron sputtering-vulcanization method, the electrostatic spinning method and other methods have the defects of complex preparation process, high equipment requirement (high cost) and the like; the direct mixing method is to mix FeS2With TiO2The method has the defects of non-uniform material and the like when the raw materials are mixed and dried in a liquid phase system.
Disclosure of Invention
In order to solve the FeS existing in the prior art2/TiO2The invention provides a pyrite iron disulfide/titanium dioxide composite material and a preparation method thereof, and solves the problems of complex preparation process, low yield, large size, agglomeration and uneven component distributionThe method and the application are that the high-purity and uniformly-mixed FeS is directly prepared in one step by a wet ball milling process2/TiO2The preparation method of the nano material is simple, protective gas does not need to be added in the reaction process, the problem of secondary pollution does not exist in the middle, the yield is high, and the TiO is2Further reduces FeS2The size of the particles. In addition, the prepared FeS2/TiO2The composite material is not combined in a pure physical sense, and the method realizes FeS2With TiO2At the same time of compounding, the doping of Fe and S elements into TiO is realized to a certain degree2In the lattice structure, the material performance is further improved.
Specifically, the invention is realized by the following technical scheme:
in a first aspect of the invention, a preparation method of a pyrite iron disulfide/titanium dioxide composite material is provided, which comprises the following steps: mixing iron powder, sulfur powder, titanium dioxide powder and wet grinding aid, ball milling, centrifuging, drying and sintering.
In a second aspect of the invention, the pyrite iron disulfide/titanium dioxide composite material prepared by the preparation method is provided.
The third aspect of the invention provides a pyrite iron disulfide/titanium dioxide composite material used as a lithium ion battery anode material, a photocatalytic degradation pollutant, a solar battery material, a photocatalytic hydrogen production by water splitting, an antibacterial agent and a photocatalytic reduction CO2Application in the field of methanol preparation.
In a fourth aspect of the invention, a lithium ion battery positive electrode material and/or a solar battery material is provided, which comprises a pyrite iron disulfide/titanium dioxide composite material.
One or more of the technical schemes have the following beneficial effects:
(1) only taking iron powder, sulfur powder and titanium dioxide powder as FeS2/TiO2The raw materials for preparing the nano composite material have simple components, wide sources and low price;
(2) the wet ball milling method is adopted to directly prepare the FeS with high purity and uniform mixing in one step2/TiO2The preparation method of the nano material is simple, protective gas does not need to be added in the reaction process, the problem of secondary pollution does not exist in the middle, the yield is high, and the requirement on equipment is not high;
(3) the method avoids the problem of agglomeration of Fe powder and S powder in the ball milling reaction process, and the pyrite type FeS is successfully prepared2And TiO is2Further reduces FeS2The particle size is 10-50 nm of the whole particle size of the composite material;
(4) the composite material prepared by the method has good mixing degree, and in addition, the prepared FeS2/TiO2The composite material is not combined in a pure physical sense, and the method realizes FeS2With TiO2At the same time of compounding, the doping of Fe and S elements into TiO is realized to a certain degree2In the lattice structure, the material performance is further improved;
(5) wet milling reaction FeS prepared according to some embodiments of the invention2/TiO2Nano-particle specific wet type ball-milling mixed FeS2With TiO2The ultraviolet light catalytic degradation performance of the sample on methylene blue is better.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a FeS prepared according to example 1 of the present invention2/TiO2Morphology picture of nanoparticles (FeS)2:TiO2＝1:2)；
FIG. 3 shows FeS prepared in example 1 of the present invention and comparative example 12/TiO2Nanoparticle XRD spectrum (FeS)2:TiO2＝1:2)；
FIG. 2 shows FeS prepared in example 2 of the present invention and comparative example 22/TiO2Nanoparticle XRD spectrum (FeS)2:TiO2＝2:1)；
FIG. 4 shows FeS prepared in example 2 of the present invention2/TiO2Nanoparticle XPS spectroscopyPicture (FeS)2:TiO2＝2:1)；
FIG. 5 shows FeS prepared in example 2 of the present invention2/TiO2Nanoparticles (named as "Wet milling reaction FeS)2/TiO2”，FeS2:TiO22:1) with wet ball milling mixed FeS2With TiO2Sample (named "wet milling mixed FeS2/TiO2”，FeS2:TiO22:1) ultraviolet photocatalytic degradation performance of methylene blue.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to solve the FeS existing in the prior art2/TiO2The invention provides a pyrite iron disulfide/titanium dioxide composite material and a preparation method and application thereof, and aims to solve the problems of complex preparation process, low yield, large size, agglomeration and uneven component distribution of the composite material2/TiO2The preparation method of the nano material is simple, protective gas does not need to be added in the reaction process, the problem of secondary pollution does not exist in the middle, the yield is high, and the TiO is2Further reduces FeS2The size of the particles. In addition, the prepared FeS2/TiO2The composite material is not combined in a pure physical sense, and the method realizes FeS2With TiO2At the same time of compounding, the doping of Fe and S elements into TiO is realized to a certain degree2In the lattice structure, the material performance is further improved.
Specifically, the invention is realized by the following technical scheme:
in a first aspect of the invention, a preparation method of a pyrite iron disulfide/titanium dioxide composite material is provided, which comprises the following steps: mixing iron powder, sulfur powder, titanium dioxide powder and wet grinding aid, ball milling, centrifuging, drying and sintering.
FeS prepared by adopting the method2/TiO2Nanoparticles, FeS2Is pyrite type iron disulfide, TiO2The composite material has an anatase structure, and the average particle size of the composite material is 10-50 nm.
With conventional FeS2/TiO2In contrast to the materials, the FeS prepared according to some embodiments of the present invention2/TiO2The material is nano-scale, the purity and the yield are high, and are respectively 92% and 80%, because on one hand, the wet grinding aid is added, so that the raw materials are mixed and contacted more uniformly while excessive cold welding and powder agglomeration are avoided in the ball-milling reaction process, and the mechanical alloying reaction efficiency is improved; secondly, the added wet grinding aid has simple components, can be completely removed by subsequent drying, heat treatment and other modes, and does not introduce other impurities; and finally, the ball milling process can be used for simply realizing mass production of products, grinding aids are added to assist in collecting ball milling product slurry after ball milling is finished, and then solid ball milling products are collected in a centrifuging, filtering and other modes, so that high collection yield can be realized.
Furthermore, conventional FeS2/TiO2The preparation method of the material is mostly to prepare FeS firstly2Then FeS is added2With TiO2The materials are combined in a liquid phase reaction or sputtering mode, and the like, and some embodiments of the invention find that the iron powder, the sulfur powder and the TiO are independent2The powder can be used for preparing FeS in one step by a ball milling mode2/TiO2In addition, the ball milling not only realizes the purpose of adding the iron powder and the sulfur powder into the TiO2The in-situ reaction on the powder surface also unexpectedly discovers iron powder and sulfurPowder with TiO2The wet grinding process of the powder is helpful to realize the doping of Fe and S elements into TiO2In the lattice structure, the material performance is further improved.
In one or more embodiments of the invention, the pyrite FeS2/TiO2The composite material is nano-scale particles.
Compared with micron-sized particles, pyrite FeS2/TiO2The composite nano-scale particles have larger specific surface area, higher transmission efficiency when being used in battery materials, and better catalytic effect when being used in the field of catalysis.
Compared with the nano tubular composite material, the iron ore FeS2/TiO2The nano-scale particles of the composite material are easier to disperse, the dispersion area is larger, and the nano-scale particles are beneficial to being uniformly distributed in the material to be modified.
In one or more embodiments of the invention, the wet grinding aid is selected from one or more of absolute ethanol, ethylene glycol.
The wet ball milling method is adopted to directly prepare the FeS with high purity and uniform mixing in one step2/TiO2The preparation method of the nano material is simple, protective gas does not need to be added in the reaction process, the problem of secondary pollution does not exist in the middle, the yield is high, and the requirement on equipment is not high.
In one or more embodiments of the invention, the ratio of the wet grinding aid dosage to the mixed powder of the iron powder, the sulfur powder and the titanium dioxide powder is as follows: 0.5 to 1 mL/g. The wet grinding aid is too much in dosage, a solution system is easily formed, ball milling or grinding is not facilitated, and the ball milling effect cannot be fully exerted. If the amount of the wet grinding aid is too small, some powder is not infiltrated by the wet grinding aid, the grinding progress is influenced, and the formation of nano FeS is not facilitated2/TiO2The nanometer material is not beneficial to doping Fe and S elements into TiO2In a lattice structure.
In one or more embodiments of the present invention, the sintering condition is 300 to 350 ℃ and the sintering time is 2 to 5 hours. The sintering aims to further optimize the wet ball milling process to prepare the pyrite FeS2Promoting a small amount of reaction intermediateFeS to pyrite2And (3) crystal phase transformation, removing a small amount of unreacted sulfur powder in the ball milling process, and further improving the purity of the composite material. The sintering temperature and time further affect the performance of the composite material by affecting the crystal structure, purity, impurity residue and the like of the ball-milled product.
Preferably, the sintering is performed in an inert atmosphere, preferably a helium, argon, nitrogen atmosphere.
In one or more embodiments of the invention, the purity of the iron powder is more than or equal to 98%, and the average particle size is 20-50 μm; the purity of the sulfur powder is more than or equal to 99.5%, and the average particle size is 20-50 mu m; the purity of the titanium dioxide powder is more than or equal to 99.8%, and the average particle size is 10-25 nm.
Preferably, the molar ratio of iron powder: and (3) sulfur powder: titanium dioxide 1: (2-2.1): x, X according to FeS2：TiO2And (4) determining a composite proportion.
Iron powder: 1, sulfur powder: (2-2.1) the object is to form FeS2A material.
In a second aspect of the invention, the pyrite iron disulfide/titanium dioxide composite material prepared by the preparation method is provided.
In one or more embodiments of the invention, the pyrite iron disulfide/titanium dioxide composite has a nanoparticle size of about 10-50 nm, and ball milling helps to homogenize the size of the composite and to distribute elements uniformly.
Preferably, the Fe and S elements are doped into TiO2In a lattice structure.
Although some methods dope Fe, S, etc. into TiO2In crystal lattices, however, their purpose is to achieve doping and not to synthesize FeS reactively2. In some embodiments of the invention, the mechanical combination energy provided by the ball milling is a power source for realizing the doping reaction, and the subsequent heat treatment process is difficult to realize the iron and sulfur in TiO according to the temperature2Doping in the crystal lattice.
The ball milling equipment for ball milling is a high-energy ball mill; preferably a planetary high energy ball mill.
The ball milling parameters of the planetary high-energy ball mill are as follows:
firstly, the diameter of the adopted zirconia ball is 3-10 mm;
secondly, according to the mass ratio, zirconia balls: the mixed material (10-30) is 1;
thirdly, the ball milling rotation speed ratio is more than or equal to 200:400 r/min;
and the ball milling time is more than or equal to 48 hours.
In some embodiments of the present invention, the ball milling time is correlated to the ball milling speed, and the corresponding ball milling time may be reduced when the speed is increased.
The third aspect of the invention provides a pyrite iron disulfide/titanium dioxide composite material used as a lithium ion battery anode material, a photocatalytic degradation pollutant, a solar battery material, a photocatalytic hydrogen production by water splitting, an antibacterial agent and a photocatalytic reduction CO2Application in the field of methanol preparation.
In a fourth aspect of the invention, a lithium ion battery positive electrode material and/or a solar battery material is provided, which comprises a pyrite iron disulfide/titanium dioxide composite material.
In a fifth aspect of the invention, a photocatalyst is provided, comprising a pyrite iron disulfide/titanium dioxide composite.
In a sixth aspect of the invention, an antimicrobial agent is provided comprising a pyrite iron disulfide/titanium dioxide composite.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
A preparation method of a pyrite iron disulfide/titanium dioxide composite material comprises the following steps:
(1) uniformly mixing iron powder, sulfur powder and titanium dioxide powder to obtain a mixed material with the total mass of 6g, wherein the iron powder comprises the following components in mol ratio: and (3) sulfur powder: titanium dioxide 1: 2: 2;
(2) adding 6mL of absolute ethyl alcohol into the mixed material, putting the mixed material into a planetary high-energy ball mill, carrying out ball milling for 48 hours, collecting ball milling product slurry by using the absolute ethyl alcohol after ball milling, centrifugally collecting powder materials, and drying to obtain FeS2/TiO2A nanocomposite material.
The ball milling parameters are as follows:
the diameter of the adopted zirconia ball is 5 mm;
secondly, according to the mass ratio, zirconia balls: the mixed material is 20: 1;
and the ball milling rotation speed ratio is 200:400 r/min.
(3) FeS dried in the previous step2/TiO2Placing the nano composite material in a vacuum tube furnace, carrying out heat treatment under the argon atmosphere to remove redundant sulfur powder, wherein the heat treatment temperature is 300 ℃, the sintering time is 2h, the argon flow rate is 100mL/min, and cooling to room temperature (25 ℃) along with the furnace to obtain FeS2/TiO2A nanocomposite material.
In the step (1), the purity of the iron powder is more than or equal to 98%, and the average particle size is 20-50 μm; the purity of the sulfur powder is more than or equal to 99.5%, and the average particle size is 20-50 mu m; the purity of the titanium dioxide powder is more than or equal to 99.8%, and the average particle size is 10-25 nm.
FIG. 1 shows FeS prepared in this example2/TiO2The shape picture of the nano particles shows that the overall size of the composite material is nano-scale, and FeS is ground2On the order of nanometers, with TiO2The nano particles are uniformly mixed, and the overall particle size of the composite material is about 10-50 nm.
Example 2
The difference from example 1 is that, in terms of molar ratio, iron powder: and (3) sulfur powder: titanium dioxide 1: 2: 0.5. the remaining parameters were the same as in example 1.
Comparative example 1
In contrast to example 1, no sintering step was carried out, i.e.
A preparation method of a pyrite iron disulfide/titanium dioxide composite material comprises the following steps:
(1) uniformly mixing iron powder, sulfur powder and titanium dioxide powder to obtain a mixed material with the total mass of 6g, wherein the iron powder comprises the following components in mol ratio: and (3) sulfur powder: titanium dioxide 1: 2: 2;
(2) adding the mixed material into 6mL of absolute ethyl alcohol, putting the mixture into a star-type high-energy ball mill, and carrying out ball milling for 48 hoursAfter grinding, collecting slurry of a ball-milling product by using absolute ethyl alcohol, centrifugally collecting a powder material, and drying to obtain FeS2/TiO2A nanocomposite material.
The ball milling parameters are as follows:
the diameter of the adopted zirconia ball is 5 mm;
fourthly, according to the mass ratio, the zirconia ball: the mixed material is 20: 1;
and the ball milling rotation speed ratio is 200:400 r/min.
In the step (1), the purity of the iron powder is more than or equal to 98%, and the average particle size is 20-50 μm; the purity of the sulfur powder is more than or equal to 99.5%, and the average particle size is 20-50 mu m; the purity of the titanium dioxide powder is more than or equal to 99.8%, and the average particle size is 10-25 nm.
Comparative example 2
The difference from comparative example 1 is that, in terms of mole ratio, iron powder: and (3) sulfur powder: titanium dioxide 1: 2: 0.5.
FeS prepared for example 1 and comparative example 1, as shown in FIG. 22/TiO2Compared with XRD spectrograms of the nano particles, XRD crystallization peaks are obvious and sharp after sintering or heat treatment, and other impurity peaks are not observed, which indicates that the product has high crystallinity and purity.
FeS prepared for example 2 and comparative example 2, as shown in FIG. 32/TiO2The XRD spectrograms of the nano particles are compared, and FeS can be known from the spectrograms2Is pyrite type iron disulfide, TiO2Has anatase structure.
FIG. 4 preparation of FeS in example 22/TiO2Nanoparticle XPS spectra (FeS)2:TiO22:1), it can be seen that the main characteristic elements in the sample are Fe, S, Ti, O, and furthermore, the method is in the realization of FeS2With TiO2At the same time of compounding, the doping of Fe and S elements into TiO is realized to a certain degree2In the lattice structure, the material performance is further improved.
FIG. 5 shows FeS prepared in example 2 of the present invention2/TiO2Nanoparticles (named as "Wet milling reaction FeS)2/TiO2”，FeS2:TiO22:1) with wet ball milling mixed FeS2With TiO2Sample (named "wet milling mixed FeS2/TiO2”，FeS2:TiO22:1) ultraviolet photocatalytic degradation performance of methylene blue.
The wet milled mixed sample was: firstly ball-milling to prepare FeS2Followed by FeS2With TiO2After mixing, wet milling was carried out under the same conditions as in example 2.
The photocatalytic experiment was: the reaction system is 200mL of 30mg/L methylene blue solution, the concentration of the catalyst is 0.3g/L, and the reaction is carried out under the irradiation of ultraviolet light
Furthermore, the catalytic degradation of methylene blue is within the 10-60min period, compared to FeS2With TiO2Physical mixing of samples, Wet milling reaction FeS prepared in example 22/TiO2The photocatalytic degradation performance is obviously improved.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a pyrite iron disulfide/titanium dioxide composite material is characterized by comprising the following steps: mixing iron powder, sulfur powder, titanium dioxide powder and wet grinding aid, ball milling, centrifuging, drying and sintering.
2. The method for preparing the pyrite iron disulfide/titanium dioxide composite according to claim 1, wherein the pyrite FeS2/TiO2The composite material is in nanometer level.
3. The method for preparing the pyrite iron disulfide/titanium dioxide composite material according to claim 1, wherein the wet grinding aid is one or more selected from absolute ethyl alcohol and ethylene glycol.
4. The preparation method of the pyrite iron disulfide/titanium dioxide composite material according to claim 1, wherein the ratio of the usage amount of the wet grinding aid to the mixed powder of the iron powder, the sulfur powder and the titanium dioxide powder is as follows: 0.5 to 1 mL/g.
5. The preparation method of the pyrite iron disulfide/titanium dioxide composite material according to claim 1, wherein the sintering condition is 300-350 ℃, and the sintering time is 2-5 h;
preferably, the sintering is in an inert atmosphere.
6. The preparation method of the pyrite iron disulfide/titanium dioxide composite material according to claim 1, wherein the purity of the iron powder is not less than 98%, and the average particle size is 20-50 μm; the purity of the sulfur powder is more than or equal to 99.5%, and the average particle size is 20-50 mu m; the purity of the titanium dioxide powder is more than or equal to 99.8%, and the average particle size is 10-25 nm;
preferably, the molar ratio of iron powder: and (3) sulfur powder: titanium dioxide 1: 2-2.1: x, X according to FeS2：TiO2And (4) determining a composite proportion.
7. The pyrite iron disulfide/titanium dioxide composite produced by the method of making the pyrite iron disulfide/titanium dioxide composite of any one of claims 1 to 6.
8. The pyrite iron disulfide/titanium dioxide composite according to claim 7, wherein the pyrite iron disulfide/titanium dioxide composite has a nanoparticle size of about 10 to 50 nm;
preferably, the Fe and S elements are doped into TiO2In a lattice structure.
9. The pyrite iron disulfide/di of claim 7 or 8Titanium oxide composite material used as anode material of lithium ion battery, photocatalytic degradation of pollutants, solar battery material, photocatalytic hydrogen production by splitting water, antibiosis and photocatalytic reduction of CO2Application in the field of methanol preparation.
10. A lithium ion battery positive electrode material and/or a solar cell material, characterized by comprising the pyrite iron disulfide/titanium dioxide composite according to claim 7 or 8.
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