CN105688943A - Method for preparing layered MoS2-TiO2 nano composite material - Google Patents
Method for preparing layered MoS2-TiO2 nano composite material Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000000463 material Substances 0.000 title claims abstract description 47
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 81
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 66
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 16
- -1 aromatic thioether Chemical class 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000002360 preparation method Methods 0.000 claims description 27
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 22
- 239000002360 explosive Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 230000001476 alcoholic effect Effects 0.000 claims description 15
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 15
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical group OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 claims description 15
- 229910052786 argon Inorganic materials 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 150000004984 aromatic diamines Chemical class 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 8
- 150000003568 thioethers Chemical class 0.000 claims description 8
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 229910052961 molybdenite Inorganic materials 0.000 abstract description 12
- 238000001914 filtration Methods 0.000 abstract description 9
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000011229 interlayer Substances 0.000 abstract description 3
- 238000003980 solgel method Methods 0.000 abstract description 2
- 238000004880 explosion Methods 0.000 abstract 5
- 238000004299 exfoliation Methods 0.000 abstract 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- 230000009920 chelation Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 229940043237 diethanolamine Drugs 0.000 abstract 1
- 238000009830 intercalation Methods 0.000 abstract 1
- 230000002687 intercalation Effects 0.000 abstract 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 29
- 229910052750 molybdenum Inorganic materials 0.000 description 29
- 239000011733 molybdenum Substances 0.000 description 26
- 239000010410 layer Substances 0.000 description 22
- 239000004408 titanium dioxide Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 13
- 239000002131 composite material Substances 0.000 description 11
- 239000012065 filter cake Substances 0.000 description 9
- 239000002356 single layer Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 238000011068 loading method Methods 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000005461 lubrication Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000005411 Van der Waals force Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000002153 concerted effect Effects 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 2
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004531 microgranule Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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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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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
- C10M125/22—Compounds containing sulfur, selenium or tellurium
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/065—Sulfides; Selenides; Tellurides
- C10M2201/066—Molybdenum sulfide
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Abstract
The invention provides a method for preparing a layered MoS2-TiO2 nano composite material. Molybdenum disulfide powder is added into a layering solution for layering reaction, filtering and drying are conducted after reaction, and layered molybdenum disulfide powder is obtained; tetrabutyl titanate, diethanol amine and absolute ethyl alcohol are mixed and then added into distilled water for chelation reaction, a precursor solution is obtained, xerogel is obtained after the precursor solution is evaporated and dried, and xerogel powder is obtained after grinding; the xerogel powder and an explosion agent are added into the layered molybdenum disulfide powder for explosion reaction, an explosion reaction product is taken out after being cooled to room temperature, and the layered MoS2-TiO2 nano composite material is obtained. The sulphophile characteristic of aromatic thioether is used, interlayer van der Waals' force of molybdenum disulfide raw material powder is reduced, and intercalation exfoliation is conducted on the molybdenum disulfide raw material powder in cooperation with explosion impact. A sol-gel method and explosion high-temperature impact are combined, quick reduction of TiO2 and exfoliation of MoS2 are completed in one step, and the layered MoS2-TiO2 nano composite material is successfully prepared.
Description
Technical field
The invention belongs to metal molybdenum technical field, relate to molybdenum bisuphide composite, be specifically related to a kind of stratiform MoS2-TiO2The preparation method of nano composite material。
Background technology
The class Graphene molybdenum bisuphide (Graphene-likeMoS being made up of monolayer or few layer molybdenum bisuphide2) it is a kind of New Two Dimensional (2D) lamellar compound with similar graphene-structured and performance, emerging study hotspot is become in recent years with the physics of its uniqueness, chemical property。The two dimensional crystal material with " sandwich " layer structure that class Graphene molybdenum bisuphide is made up of the single or multiple lift molybdenum bisuphide of hexagonal crystal system, monolayer molybdenum bisuphide is made up of three layers atomic layer, middle one layer is molybdenum atom layer, upper and lower two-layer is sulphur atom layer, molybdenum atom layer forms class " sandwich " structure folded by two-layer sulphur atom layer, and molybdenum atom is combined formation two-dimensional atomic crystal with sulphur atom with covalent bond；Multilamellar molybdenum bisuphide is made up of some monolayer molybdenum bisuphide, is usually no more than five layers, and interlayer exists weak Van der Waals force, and interlamellar spacing is about 0.65nm。
It is widely used in various fields such as lubricant, catalysis, energy storage, composites with " sandwich " layer structure of its uniqueness as the two-dimensional layer nano material that a class is important, monolayer or few layer molybdenum bisuphide。Compared to zero band gap of Graphene, there is regulatable band gap in class Graphene molybdenum bisuphide, has brighter prospect at field of photoelectric devices；Said three-dimensional body phase structure compared to silicon materials, class Graphene molybdenum bisuphide has the two-dimensional layered structure of nanoscale, can be used to manufacture quasiconductor or specification is less, efficiency is higher electronic chip, will be used widely in fields such as follow-on nano-electric devices。
Although platelike molybdenumdisulfide has good greasy property and photoelectric properties, but it needs to be further improved in all many-sided performances, by molybdenum bisuphide with other organic or inorganic microgranule compound use, utilize their cooperative effect, be an up one of method of molybdenum bisuphide performance。Titanium dioxide has the photocatalysis performance of excellence, is one of conventional photocatalyst, additionally, titanium dioxide also has certain greasy property。Research shows, there is collaborative lubrication and concerted catalysis effect in titanium dioxide and molybdenum bisuphide, it is one of the lubrication improving molybdenum bisuphide and the titanium dioxide effective way with catalytic performance (TribologyLetters by chemical method synthesis of carbon/molybdenum disulfide-titanium dioxide compound, 2011,43:77-87)。
Chinese invention patent CN201410369695 discloses a kind of molybdenum bisuphide-titanium dioxide compound and preparation method thereof, utilize titanium dioxide and the collaborative lubrication of molybdenum bisuphide existence and concerted catalysis effect, be one of the lubrication improving molybdenum bisuphide and titanium dioxide effective way with catalytic performance by chemical method synthesis of carbon/molybdenum disulfide-titanium dioxide compound；Chinese invention patent ZL201010524516.8 adds a certain amount of titanium dioxide when molybdate reacts under strongly acidic conditions with thioacetamide, utilize the strong acid activation titanium dioxide surface of reaction system, the titanium dioxide surface of activation is provided that more core being available for presoma precipitation, thus forerunner's physical ability is deposited in the surface of titanium dioxide fine particles in a short period of time, form the molybdenum bisuphide-titanium dioxide compound of spherical structure；And if replace thioacetamide above with sodium sulfide, what reaction generated is then the molybdenum bisuphide-titanium dioxide compound (JournalofMaterialsScience, 2010,45:2640-2648) of laminated structure。
Although mean disclosed above adopts chemical synthesis to prepare MoS2-TiO2Nano composite material, but its preparation flow is complicated, and energy consumption is big, is not suitable for industrialized production, and is graininess MoS for adopting raw material2Prepare laminar composite and do not propose effective workaround, and for the MoS of rich in mineral resources2Material, rationalizes it, higher value application is the trend of at present development。Therefore, explore one and adopt granule MoS2Stratiform MoS is prepared for raw material2-TiO2The simple and easy method of nano composite material is very necessary。
Summary of the invention
Based on problems of the prior art, the present invention proposes a kind of stratiform MoS2-TiO2The preparation method of nano composite material, it is thus achieved that there is the stratiform MoS of nanoscale, superior performance2-TiO2Nano composite material, solves existing MoS2-TiO2Composite preparation flow is complicated, and energy consumption is big, is not suitable for industrialized production, and makes photocatalysis and the poor technical problem of greasy property for graininess。
It should be noted that the stratiform MoS in the application2-Fe3O4MoS in nano composite material2It is monolayer or few layer MoS2Nano material, described few layer refers to 2 layers to 5 layers。
In order to solve above-mentioned technical problem, the application adopts the following technical scheme that and is achieved:
A kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction in layering solution, filter, dry after having reacted, obtain layering molybdenum disulfide powder；
Step 2, adds in distilled water after butyl titanate, diethanolamine being mixed with dehydrated alcohol, carries out chelatropic reaction, obtain precursor solution, obtains xerogel after precursor solution evaporation drying, grinds and obtains dry gel powder；
Step 3, adds dry gel powder and burster in layering molybdenum disulfide powder, carries out explosive reaction, takes out explosive reaction product, namely obtain stratiform MoS after being cooled to room temperature2-TiO2Nano composite material。
The present invention also has and distinguishes technical characteristic as follows:
Described layering solution is the alcoholic solution of aromatic thioether；Described burster is picric acid。
Described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, and the mass concentration of the alcoholic solution of aromatic thioether is 10%～60%。
In step one, the detailed process of described layering reaction is: molybdenum disulfide powder is ground to 200 orders and sieves, added by molybdenum disulfide powder in the alcoholic solution of aromatic thioether, heating is to 30～70 DEG C and stirs 5～12h, filter, dry, obtain layering molybdenum disulfide powder。
In step one, the mass ratio of described molybdenum disulfide powder and aromatic thioether is 1:(10～40)。
In step 2, the detailed process of chelatropic reaction is: add in distilled water after butyl titanate, diethanolamine being mixed with dehydrated alcohol, precursor solution is obtained after stirring chelating 3～10h at 45～80 DEG C, precursor solution is obtained after evaporation drying 6～15h at 100～130 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
In step 2, the mass volume ratio of described described butyl titanate, diethanolamine, dehydrated alcohol and distilled water is 1g:(10～20) ml:(15～30) ml:(5～20) ml。
In step 3, the detailed process of described explosive reaction is: will be layered molybdenum disulfide powder, dry gel powder and picric acid mix homogeneously, load in autoclave, by autoclave evacuation and pass into argon, heating is blasted to 350～600 DEG C, take out explosive reaction thing after cooling to room temperature with the furnace, namely obtain stratiform MoS2-TiO2Nano composite material。
In step 3, the described mass ratio being layered molybdenum disulfide powder, dry gel powder and picric acid mixing is 1:(0.5～5): (0.5～3)。
Compared with prior art, useful has the technical effect that the present invention
(I) present invention utilizes the close sulphur property of aromatic thioether, reduces the interlayer Van der Waals force of molybdenum bisuphide material powder, in conjunction with blast impulse, it is carried out delamination。
(II) present invention is combined with blast high temperature impact by sol-gel process, only namely completes TiO by a step2Rapidly reduction and MoS2Stripping, be successfully prepared stratiform MoS2-TiO2Nano composite material。
(II) product prepared by the present invention is platelike molybdenumdisulfide and the TiO with high carrier mobility2The nano material of nano-particles reinforcement, and TiO2Nano-particle is uniformly attached on monolayer molybdenum bisuphide lamella, improves its catalysis and greasy property, is greatly expanded the range of application of molybdenum bisuphide。
(IV) present invention prepares stratiform MoS2-TiO2Nano composite material, simple to operate, it is not necessary to complicated and loaded down with trivial details preparation facilities, preparation efficiency is high, and yield is big, is suitable for industrialized production。
Accompanying drawing explanation
Fig. 1 is the stratiform MoS in embodiment 12-TiO2The Raman collection of illustrative plates of nano composite material。
Fig. 2 is the stratiform MoS in embodiment 12-TiO2The TEM figure of nano composite material。
Fig. 3 is the MoS in comparative example 12-TiO2The Raman collection of illustrative plates of composite。
Fig. 4 is the MoS in comparative example 12-TiO2The TEM figure of composite。
Below in conjunction with drawings and Examples, the particular content of the present invention is described in more detail。
Detailed description of the invention
Defer to technique scheme, specific embodiments of the invention given below, it is necessary to explanation is to the invention is not limited in specific examples below, and all equivalents done on technical scheme basis each fall within protection scope of the present invention。Below in conjunction with embodiment, the present invention is described in further details。
Embodiment 1:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 10%, in alcoholic solution containing 100g polyphenylene sulfide, heating in water bath is to 30 DEG C and stirs 12h, filter and filter cake is dried, be ground to 200 orders and sieve, obtain 3.1g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 50ml diethanolamine adds in 25ml distilled water after mixing with 75ml dehydrated alcohol, precursor solution is obtained after stirring chelating 3h at 45 DEG C, precursor solution is obtained after dry 6h at 100 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 3.1g is layered molybdenum disulfide powder with 1.6g dry gel powder, 1.6g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 500 DEG C, take out explosive reaction thing deionized water after cooling to room temperature with the furnace repeatedly to rinse, after filtration drying, namely obtain stratiform MoS2-TiO2 nano composite material。
Stratiform MoS prepared by the present embodiment2-TiO2Nano composite material Raman collection of illustrative plates is as it is shown in figure 1, high-resolution TEM schemes as shown in Figure 2。
E in Raman collection of illustrative plates in Fig. 12g 1With Ag 1Value respectively 384.06 and 406.91, displacement difference is 22.85, belongs to few Rotating fields MoS2, it was shown that MoS in sample prepared by the present embodiment2For stratified material。
Fig. 2 middle high-resolution TEM figure is shown as TiO2Nano-particle attachment MoS2Laminar nano chip architecture surface。
Comprehensive accompanying drawing can show that the sample prepared by the present embodiment is stratiform MoS2-TiO2Nano composite material。
Embodiment 2:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 20%, in alcoholic solution containing 200g polyphenylene sulfide, heating in water bath is to 50 DEG C and stirs 5h, filter and filter cake is dried, be ground to 200 orders and sieve, obtain 3.4g and be layered molybdenum disulfide powder；
Step 2, take 5g butyl titanate, 75ml diethanolamine adds in 50ml distilled water after mixing with 100ml dehydrated alcohol, precursor solution is obtained after stirring chelating 4h at 50 DEG C, precursor solution is obtained after dry 7h at 105 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 3.4g is layered molybdenum disulfide powder with 3.4g dry gel powder, 3.4g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 480 DEG C, explosive reaction thing is taken out after cooling to room temperature with the furnace, repeatedly rinse with deionized water, after filtration drying, namely obtain stratiform MoS2-TiO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-TiO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 3:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, takes 10g molybdenum disulfide powder and is ground to 200 orders and sieves, be added into mass concentration be 30%, in alcoholic solution containing 300g polyphenylene sulfide, heating in water bath is to 40 DEG C and stirs 8h, filter and filter cake is dried, be ground to 200 orders and sieve, obtain 2.8g and be layered molybdenum disulfide powder；
Step 2, take 5g butyl titanate, 100ml diethanolamine adds in 75ml distilled water after mixing with 125ml dehydrated alcohol, precursor solution is obtained after stirring chelating 5h at 60 DEG C, precursor solution is obtained after dry 9h at 110 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 2.8g is layered molybdenum disulfide powder with 4.5g dry gel powder, 5.6g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 450 DEG C, take out explosive reaction thing deionized water after cooling to room temperature with the furnace repeatedly to rinse, after filtration drying, namely obtain stratiform MoS2-TiO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-TiO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 4:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 40%, in alcoholic solution containing 400g aromatic diamine monomer thioether, heating in water bath is to 35 DEG C and stirs 10h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 3.2g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 50ml diethanolamine adds in 100ml distilled water after mixing with 150ml dehydrated alcohol, precursor solution is obtained after stirring chelating 6h at 65 DEG C, precursor solution is obtained after dry 11h at 115 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 3.2g is layered molybdenum disulfide powder with 6.4g dry gel powder, 1.6g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 550 DEG C, take out explosive reaction thing deionized water after cooling to room temperature with the furnace repeatedly to rinse, ultrasonic disperse 6h, namely obtains stratiform MoS after filtration drying2-TiO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-TiO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 5:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 60%, in alcoholic solution containing 300g aromatic diamine monomer thioether, heating in water bath is to 30 DEG C and stirs 12h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 2.6g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 50ml diethanolamine adds in 75ml distilled water after mixing with 100ml dehydrated alcohol, precursor solution is obtained after stirring chelating 8h at 70 DEG C, precursor solution is obtained after dry 13h at 120 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, is layered molybdenum disulfide powder and 10gTiO by gained 2.6g2Nanometer powder, 2.6g picric acid are pressed mix homogeneously and are loaded in autoclave, evacuation also passes into argon, reactor heating is blasted to 510 DEG C, takes out explosive reaction thing deionized water after cooling to room temperature with the furnace and repeatedly rinse, after filtration drying, namely obtain stratiform MoS2-TiO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-TiO2The character of nano composite material is substantially the same manner as Example 1。
Embodiment 6:
The present embodiment provides a kind of stratiform MoS2-TiO2The preparation method of nano composite material, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 50%, in alcoholic solution containing 200g aromatic diamine monomer thioether, heating in water bath is to 45 DEG C and stirs 8h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 3.3g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 100ml diethanolamine adds in 50ml distilled water after mixing with 75ml dehydrated alcohol, precursor solution is obtained after stirring chelating 10h at 80 DEG C, precursor solution is obtained after dry 15h at 110 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, is layered molybdenum disulfide powder and 16.5gTiO by gained 3.3g2Nanometer powder, 5.4g picric acid are pressed mix homogeneously and are loaded in autoclave, evacuation also passes into argon, reactor heating is blasted to 500 DEG C, takes out explosive reaction thing deionized water after cooling to room temperature with the furnace and repeatedly rinse, after filtration drying, namely obtain stratiform MoS2-TiO2Nano composite material。
The present embodiment products therefrom stratiform MoS2-TiO2The character of nano composite material is substantially the same manner as Example 1。
Comparative example 1:
This comparative example provides a kind of MoS2-TiO2The preparation method of composite, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 5%, in alcoholic solution containing 50g aromatic diamine monomer thioether, heating in water bath is to 25 DEG C and stirs 5h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 3.2g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 20ml diethanolamine adds in 20ml distilled water after mixing with 50ml dehydrated alcohol, precursor solution is obtained after stirring chelating 2h at 40 DEG C, precursor solution is obtained after dry 8h at 90 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 3.2g is layered molybdenum disulfide powder with 0.5g dry gel powder, 1g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 600 DEG C, take out explosive reaction thing deionized water after cooling to room temperature with the furnace repeatedly to rinse, after filtration drying, obtain MoS2-TiO2Complex。
The MoS that this comparative example is prepared2-TiO2Complex carries out Raman spectrum analysis and tem analysis。
Raman spectrum is as it is shown on figure 3, its E2g 1With Ag 1Value respectively 381.65 and 406.91, displacement difference is 25.26, belongs to block structure MoS2。
TEM image as shown in Figure 4, illustrates this product MoS2Block is piled up, and presents multiple structure, and at MoS2Surface or surrounding do not find obvious TiO2Granule, is not belonging to monolayer or few layer MoS2Nano composite material。
Comparative example 2:
This comparative example provides a kind of MoS2-TiO2The preparation method of composite, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 70%, in alcoholic solution containing 500g aromatic diamine monomer thioether, heating in water bath is to 60 DEG C and stirs 4h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 3g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 50ml diethanolamine adds in 100ml distilled water after mixing with 20ml dehydrated alcohol, precursor solution is obtained after stirring chelating 3h at 90 DEG C, precursor solution is obtained after dry 5h at 100 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, is layered molybdenum disulfide powder and 18gTiO by gained 3g2Nanometer powder, 0.5g picric acid are pressed mix homogeneously and are loaded in autoclave, and evacuation also passes into argon, reactor heating are blasted to 650 DEG C, take out explosive reaction thing deionized water and repeatedly rinse, obtain MoS after filtration drying after cooling to room temperature with the furnace2-TiO2Complex。
The MoS that this comparative example prepares2-TiO2Composite block the same as comparative example 1 is piled up, and TiO2Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano-composite material。
Comparative example 3:
This comparative example provides a kind of MoS2-TiO2The preparation method of composite, the method specifically includes following steps:
Step one, take 10g molybdenum disulfide powder to be ground to 200 orders and sieve, be added into mass concentration be 8%, in alcoholic solution containing 60g aromatic diamine monomer thioether, heating in water bath is to 25 DEG C and stirs 5h, filter and filter cake is dried, it is ground to 200 orders to sieve, obtains 3.5g and be layered molybdenum disulfide powder。
Step 2, take 5g butyl titanate, 100ml diethanolamine adds in 150ml distilled water after mixing with 10ml dehydrated alcohol, precursor solution is obtained after stirring chelating 4h at 85 DEG C, precursor solution is obtained after dry 4h at 110 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
Step 3, gained 3.5g being layered molybdenum disulfide powder with 1.5g dry gel powder, 1.5g picric acid by mixing homogeneously in loading autoclave, evacuation also passes into argon, reactor heating is blasted to 620 DEG C, take out explosive reaction thing after cooling to room temperature with the furnace, obtain MoS2-TiO2Complex。
The MoS that this comparative example prepares2-TiO2Composite block the same as comparative example 1 is piled up, and TiO2Granule occurs in MoS2Block surface and surrounding, be not belonging to monolayer or few layer molybdenum disulfide nano-composite material。
Claims (9)
1. a stratiform MoS2-TiO2The preparation method of nano composite material, it is characterised in that: the method comprises the following steps:
Step one, adds molybdenum disulfide powder and carries out layering reaction in layering solution, filter, dry after having reacted, obtain layering molybdenum disulfide powder；
Step 2, adds in distilled water after butyl titanate, diethanolamine being mixed with dehydrated alcohol, carries out chelatropic reaction, obtain precursor solution, obtains xerogel after precursor solution evaporation drying, grinds and obtains dry gel powder；
Step 3, adds dry gel powder and burster in layering molybdenum disulfide powder, carries out explosive reaction, takes out explosive reaction product, namely obtain stratiform MoS after being cooled to room temperature2-TiO2Nano composite material。
2. preparation method as claimed in claim 1, it is characterised in that: described layering solution is the alcoholic solution of aromatic thioether；Described burster is picric acid。
3. preparation method as claimed in claim 2, it is characterised in that: described aromatic thioether is polyphenylene sulfide or aromatic diamine monomer thioether, and the mass concentration of the alcoholic solution of aromatic thioether is 10%～60%。
4. preparation method as claimed in claim 2, it is characterized in that: in step one, the detailed process of described layering reaction is: molybdenum disulfide powder is ground to 200 orders and sieves, molybdenum disulfide powder is added in the alcoholic solution of aromatic thioether, heating is to 30～70 DEG C and stirs 5～12h, filter, dry, obtain layering molybdenum disulfide powder。
5. preparation method as claimed in claim 2, it is characterised in that: in step one, the mass ratio of described molybdenum disulfide powder and aromatic thioether is 1:(10～40)。
6. preparation method as claimed in claim 2, it is characterized in that: in step 2, the detailed process of chelatropic reaction is: add in distilled water after butyl titanate, diethanolamine being mixed with dehydrated alcohol, precursor solution is obtained after stirring chelating 3～10h at 45～80 DEG C, precursor solution is obtained after evaporation drying 6～15h at 100～130 DEG C xerogel, and is ground to 200 orders and sieves and obtain dry gel powder。
7. preparation method as claimed in claim 2, it is characterized in that: in step 2, the mass volume ratio of described described butyl titanate, diethanolamine, dehydrated alcohol and distilled water is 1g:(10～20) ml:(15～30) ml:(5～20) ml。
8. preparation method as claimed in claim 2, it is characterized in that: in step 3, the detailed process of described explosive reaction is: will be layered molybdenum disulfide powder, dry gel powder and picric acid mix homogeneously, load in autoclave, by autoclave evacuation and pass into argon, heating is blasted to 350～600 DEG C, takes out explosive reaction thing, namely obtain stratiform MoS after cooling to room temperature with the furnace2-TiO2Nano composite material。
9. preparation method as claimed in claim 2, it is characterised in that: in step 3, the described mass ratio being layered molybdenum disulfide powder, dry gel powder and picric acid mixing is 1:(0.5～5): (0.5～3)。
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