CN106964368A - A kind of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials and preparation method thereof - Google Patents
A kind of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials and preparation method thereof Download PDFInfo
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- CN106964368A CN106964368A CN201710169240.8A CN201710169240A CN106964368A CN 106964368 A CN106964368 A CN 106964368A CN 201710169240 A CN201710169240 A CN 201710169240A CN 106964368 A CN106964368 A CN 106964368A
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- titanium dioxide
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- fiber composite
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- nanometer sheet
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 320
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 154
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 137
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 137
- 239000010439 graphite Substances 0.000 title claims abstract description 137
- 239000000835 fiber Substances 0.000 title claims abstract description 136
- 239000002055 nanoplate Substances 0.000 title claims abstract description 133
- 239000002131 composite material Substances 0.000 title claims abstract description 103
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000001699 photocatalysis Effects 0.000 claims abstract description 38
- 238000007146 photocatalysis Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000013049 sediment Substances 0.000 claims description 51
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 38
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 30
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 18
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 11
- 238000013019 agitation Methods 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 229910003087 TiOx Inorganic materials 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 claims description 2
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 239000002135 nanosheet Substances 0.000 claims 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 9
- 229940012189 methyl orange Drugs 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 235000010215 titanium dioxide Nutrition 0.000 description 136
- 229960005196 titanium dioxide Drugs 0.000 description 130
- 238000000926 separation method Methods 0.000 description 8
- 239000011684 sodium molybdate Substances 0.000 description 8
- 235000015393 sodium molybdate Nutrition 0.000 description 8
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 8
- 241000209094 Oryza Species 0.000 description 7
- 235000007164 Oryza sativa Nutrition 0.000 description 7
- 235000009566 rice Nutrition 0.000 description 7
- 239000003643 water by type Substances 0.000 description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 5
- 230000008859 change Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000002023 wood Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- PMUIBVMKQVKHBE-UHFFFAOYSA-N [S].NC(N)=O Chemical compound [S].NC(N)=O PMUIBVMKQVKHBE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- AQRDGTBNWBTFKJ-UHFFFAOYSA-N molybdenum;dihydrate Chemical compound O.O.[Mo] AQRDGTBNWBTFKJ-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials and preparation method thereof, two-dimentional molybdenum sulfide nanometer sheet, the 3-D heterojunction structure enhancing titanium dioxide nanoplate visible light photocatalysis effect that two-dimentional titanium dioxide nanoplate is constituted with one-dimensional graphite fibre, realize ultraviolet light, excellent photocatalysis effect is respectively provided with visible ray, so as to widen the utilization scope to sunshine, improve photocatalysis effect, this method molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are in ultraviolet light, higher photocatalysis efficiency is respectively provided with visible ray to methyl orange, effectively increase the utilization rate to sunshine and operating process of the present invention is simple, production cost is low, it is easy to spread, application of the titanium dioxide in actual photocatalysis field is greatly facilitated.
Description
Technical field
The present invention relates to photochemical catalyst field, and in particular to a kind of to have ultraviolet and visible light photocatalysis effect molybdenum sulfide
Nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials and preparation method thereof.
Background technology
Photocatalysis field is developed rapidly in recent years, and photocatalytic degradation organic matter is even more one of photocatalysis research field important
Branch.Photocatalysis technology, is the chemical reaction carried out in the presence of light.Photochemical reaction needs molecule absorption specific wavelength
Electromagnetic radiation, is excited to produce molecular-excited state, then can occur the new material of chemical reaction generation, or become to trigger thermal response
Middle chemical product.Photochemically reactive activation energy derive from photon energy, in the utilization of solar energy photoelectric conversion with
And photochemical transformation always very active research field.
Using optically catalytic TiO 2 degradating organic dye, not only efficiency high, cost are low but also environmentally friendly reliable.Titanium dioxide
Photochemical catalyst turns into the photochemical catalyst commonly used because catalytic activity is high, oxidability is strong, stability is good, reaction condition is gentle etc..But
It is that titanium dioxide belongs to wide bandgap semiconductor, and the energy gap of titanium dioxide is 3.2eV, and 380nm purple can only be less than by wavelength
Outer light, which is excited, makes titanium dioxide occur electron transition, so as to produce electron-hole pair.And in sunshine spatial distribution only about
There is 5% ultraviolet light, it is seen that the energy of light accounts for 48%, and titanium dioxide can not produce response to remaining most of visible ray.
In addition, when titanium dioxide is by solar radiation, the electron-hole pair excited by sunshine is easy to multiple rapidly internally
Close, this hinders application of the titanium dioxide in actual photocatalysis field significantly.
At present, prepared usually through modifying titanium dioxide with visible light catalysis activity photochemical catalyst.Such as Publication No.
CN101596457A discloses the nano titanium dioxide photocatalyst of a kind of boron and other elements codope, and the titanium-dioxide photo is urged
Boron and other elements are doped with agent, the other elements can be in transition metal, rare earth metal or nonmetalloid
It is one or more.But the photocatalysis efficiency of the patent is low, application is narrower.
Graphite fibre is that graphitization, phosphorus content have stratiform hexagoinal lattice graphite-structure to molecular structure higher than 99%
Fiber.Graphite fibre has the electric conductivity of high-quality, is good electron acceptor, the electricity of titanium dioxide is compensate for a certain extent
Son-hole easily compound defect.Titanium dioxide nanoplate has higher proportion of { 001 } active crystal face, has in photocatalytic degradation
It is dominant during organic pollutants, with reference to two-dimentional molybdenum sulfide nanometer sheet, two-dimentional titanium dioxide nanoplate and one-dimensional graphite fibre
The 3-D heterojunction structure of composition can strengthen titanium dioxide nanoplate photocatalysis effect, make up the deficiency of titanium dioxide nanoplate.It is existing
Have and be not related to two-dimentional molybdenum sulfide nanometer sheet, three that two-dimentional titanium dioxide nanoplate is constituted with one-dimensional graphite fibre in technology also
Tieing up heterojunction structure strengthens the relevant report of titanium dioxide nanoplate visible light photocatalysis effect.
The content of the invention
The present invention for solve that existing photocatalysis material of titanium dioxide is present can only to absorb ultraviolet light, photocatalysis efficiency low
Technical problem, an object of the present invention be to provide it is a kind of have ultraviolet and visible light photocatalysis effect, photocatalysis efficiency
High molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials.Molybdenum sulfide nanometer sheet/the nano titania
In piece/graphite fiber composite materials the thickness of the titanium dioxide nanoplate of liquid growth be 75~100nm, width be 700~
1000nm, molybdenum sulfide nanometer sheet is covered in titanium dioxide nanoplate surface in stratiform.
The second object of the present invention is to provide a kind of high with ultraviolet and visible light photocatalysis effect, photocatalysis efficiency
The preparation method of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials.Obtain a kind of molybdenum sulfide nanometer sheet/
Titanium dioxide nanoplate/graphite fiber composite materials operating process is simple, the low preparation technology of production cost.
To solve above technical problem, the present invention provides following technical scheme：
A kind of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials, molybdenum sulfide nanometer sheet/bis-
The thickness of the titanium dioxide nanoplate of liquid growth is 75~100nm, width in TiOx nano piece/graphite fiber composite materials
For 700~1000nm, molybdenum sulfide nanometer sheet is covered in titanium dioxide nanoplate surface in stratiform.
A kind of preparation method of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials, specific steps are such as
Under：
Step 1：After a certain amount of graphite fibre, hydrochloric acid solution are mixed, it is added dropwise after ultrasonic reaction grinding a certain amount of
Butyl titanate, hydrogen fluoride solution are sufficiently stirred for preparing the first reaction solution.
Step 2：First mixed liquor is placed in hydrothermal reaction kettle, fully product is filtered after reaction, clean, dries preparation
Into titanium dioxide nanoplate/graphite fiber composite materials.
Step 3：A certain amount of titanium dioxide nanoplate/graphite fiber composite materials are taken to add appropriate Sodium Molybdate Dihydrate and sulphur
Urea, the second reaction solution is made into deionized water.
Step 4：Second mixed liquor is placed in hydrothermal reaction kettle after fully reaction product is filtered respectively, cleaned, is dried
Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are made.
Titanium dioxide nanoplate/graphite fiber composite materials prepared by step 2 promote the separation in light induced electron and hole,
Effectively increase the utilization rate to sunshine, this method molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite prepared by step 4
Fibrous composite is respectively provided with higher photocatalytic degradation effect under ultraviolet light, visible ray to methyl orange, effectively increases pair
The utilization rate of sunshine, the three-dimensional that two-dimentional molybdenum sulfide nanometer sheet, two-dimentional titanium dioxide nanoplate are constituted with one-dimensional graphite fibre
Heterojunction structure can strengthen titanium dioxide nanoplate photocatalysis effect, make up the deficiency of titanium dioxide nanoplate.
It is preferred that, the concrete operations of step 1 be take 18 milliliters, 5 moles every liter of hydrochloric acid solution fills with 0.3 gram of graphite fibre
Divide and mix 10 minutes, be added dropwise dropwise after butyl titanate, solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, then by
0.35 milliliter of mass fraction is added dropwise to be stirred 5 minutes after 47% hydrofluoric acid in drop, produces mixed liquor.
It is preferred that, the addition of butyl titanate is 0.5-1.5 milliliters in step 1.
It is furthermore preferred that the addition of butyl titanate is 1.0 milliliters in step 1.
It is preferred that, the hydrothermal reaction condition of step 2：180 DEG C of reaction temperature, the reaction time is 4 hours.
It is preferred that, the concrete operations of the cleaning process of step 2 are：With aqueous isopropanol (deionized water and isopropanol volume
Than for 2:1) it is cleaned by ultrasonic 3 minutes, then the sediment after washing is cleaned with 0.1 mole every liter of sodium hydroxide solution, obtained
To sediment neutrality is washed with deionized water again.
It is preferred that, the drying process of step 2 is：Taken out after being dried 12 hours under conditions of 60 DEG C.
It is preferred that, titanium dioxide nanoplate/graphite fiber composite materials addition described in step 3 is 50 milligrams, is gone
Ionized water addition is 20 milliliters.
It is preferred that, Sodium Molybdate Dihydrate described in step 3 is 1 with the mass ratio that thiocarbamide is added：2.
It is preferred that, the Sodium Molybdate Dihydrate quality added in step 3 is 6-42 milligrams.
Most preferably, Sodium Molybdate Dihydrate and thiocarbamide addition are respectively 18 milligrams and 36 milligrams in step 3.
It is preferred that, the hydrothermal reaction condition of step 4：200 DEG C of reaction temperature, 24 hours reaction time.
It is preferred that, the cleaning of step 4, drying process are：Cleaned with deionized water, the drying temperature is 50 DEG C, institute
Drying time is stated for 12h.
Present invention also offers a kind of catalysis material, the catalysis material includes graphite fibre matrix and positioned at graphite
The titanium dioxide nanoplate on fibrous matrix surface and the molybdenum sulfide nanometer sheet photocatalysis material for loading to titanium dioxide nanoplate surface
Material；Wherein, the catalysis material is compound for molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fibre of the present invention
Material.
Beneficial effects of the present invention：
(1) molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials prepared by the present invention effectively facilitate light
The separation of raw electron hole, two-dimentional molybdenum sulfide nanometer sheet, two-dimentional titanium dioxide nanoplate and the three of one-dimensional graphite fibre composition
Tie up heterojunction structure enhancing titanium dioxide nanoplate visible light photocatalysis effect, realize be respectively provided with ultraviolet light, visible ray it is excellent
Photocatalysis effect, so as to widen the utilization scope to sunshine, improves photocatalysis effect.
(2) present invention prepares molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials by hydro-thermal method,
Compared with the titanium dioxide nanoplate of single structure, titanium dioxide nanoplate prepared by this method/graphite fiber composite materials promote
Enter the separation in light induced electron and hole, effectively increase the utilization rate to sunshine.Compared with independent titanium dioxide nanoplate,
This method molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are equal to methyl orange under ultraviolet light, visible ray
With higher photocatalysis efficiency, the utilization rate to sunshine is effectively increased.
(3) operating process of the present invention is simple, and production cost is low, it is easy to promote, and titanium dioxide is greatly facilitated in actual light
The application of catalytic field.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of obtained titanium dioxide nanoplate/graphite fiber composite materials in embodiment 5.
Fig. 2 is that obtained molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are swept in embodiment 5
Retouch electron microscope.
Fig. 3 is obtained titanium dioxide nanoplate/graphite fiber composite materials in embodiment 3,5 respectively in ultraviolet light
Under to the photocatalytic activity and the change curve of time of methyl orange solution.
Fig. 4 is obtained molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials in embodiment 4,5,6
Photocatalytic activity and the change curve of time under ultraviolet light and radiation of visible light to methyl orange solution respectively.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
The present invention is further described with reference to the accompanying drawings and examples, in order to the understanding of technical staff of the same trade：
The surface topography test of the mixed powder of embodiment 1 is carried out using SEM, specific test result is shown in
Fig. 1.
The raw material that following embodiments 1 are used into embodiment 6 is graphite fibre, butyl titanate, hydrochloric acid, hydrofluoric acid, two water
Sodium molybdate, thiocarbamide and deionized water.
Used equipment has the beaker for mixing, magnetic stirring apparatus, hydrothermal reaction kettle, baking oven etc..
When producing molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials, first by graphite fibre and salt
Acid is sufficiently mixed the first mixed liquor of preparation, then adds butyl titanate to the first mixed liquor and stirs the second mixed liquor of preparation；So
Hydrofluoric acid is added in backward second mixed liquor to be sufficiently stirred for preparing the 3rd mixed liquor；The 3rd mixed liquor is subsequently put into hydro-thermal anti-
Reaction in kettle is answered to produce the 4th mixed liquor；Then the 4th mixed liquor is filtrated to get sediment, the sediment being separated to first is used
Isopropanol is cleaned by ultrasonic and then washed with sodium hydroxide, and neutrality is finally washed with deionized water, and obtained sediment is dried and made
Obtain titanium dioxide nanoplate/graphite fiber composite materials；By titanium dioxide nanoplate/graphite fiber composite materials, molybdate dihydrate acid
Sodium and thiocarbamide produce the 5th mixed liquor in being sufficiently mixed in deionized water；Then the 5th mixed liquor is put into hydrothermal reaction kettle
The 6th mixed liquor is produced in reaction；Then the 6th mixed liquor is filtrated to get sediment, finally washing by the sediment being separated to simultaneously
Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are made in drying.Take out obtained nano titania
Piece/graphite fiber composite materials and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are also needed by scanning
Electronic Speculum and photocatalysis effect test system carry out observation analysis.
A kind of preparation side for molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials that the present invention is provided
Method, is comprised the following steps that：
The first step：0.3 gram of graphite fibre is taken, is added in 18 milliliters, 5 moles every liter of hydrochloric acid solution, ultrasound 10 minutes
Prepare the first mixed liquor.
Second step：3 part of first mixed liquor is taken, same amount butyl titanate is added dropwise in 3 part of first mixed liquor respectively,
It is sufficiently stirred for preparing the second mixed liquor in 30 minutes.
3rd step：The hydrogen fluoride solution that 0.35 milliliter of mass fraction is 47% is added into the second mixed liquor respectively, fully
Stirring prepares the 3rd mixed liquor in 5 minutes.
4th step：3rd mixed liquor is placed in hydrothermal reaction kettle, fully reaction 4 hours, prepares the under the conditions of 180 DEG C
Four mixed liquors.
5th step：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, it is then that the sediment after washing is molten with 0.1 mole every liter of sodium hydroxide
Liquid is cleaned, and neutrality is washed with deionized water in obtained sediment again, is dried under conditions of 60 DEG C 12 hours, is finally taken out and prepare
Into titanium dioxide nanoplate/graphite fiber composite materials.
6th step：Take 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials, add not same amount Sodium Molybdate Dihydrate with
Thiocarbamide, the 5th mixed liquor of different proportion is made into 20 ml deionized waters.
7th step：5th mixed liquor is placed in hydrothermal reaction kettle, fully reacted 24 hours under the conditions of 200 DEG C, is prepared
6th mixed liquor.
8th step：Filter the 6th mixed liquor and obtain sediment, obtained sediment is cleaned with deionized water, at 50 DEG C
Under the conditions of dry 12 hours, finally take out the molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials being made.
Embodiment 1
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 0.5 milliliter of butyl titanate is measured, butyl titanate is added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 18 milligram two is then weighed
Water sodium molybdate, then 36 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
It is added in 20 ml deionized waters and fully dissolving prepares the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials, have grown pole on graphite fibre made from above-described embodiment 1
A small amount of titanium dioxide nanoplate.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fibre is multiple made from above-described embodiment 1
Condensation material, stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.With titanium dioxide nanoplate/graphite fibre
Composite is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are right under ultraviolet light, visible ray
Methyl orange is respectively provided with higher photocatalysis efficiency, effectively increases the utilization rate to sunshine.
Embodiment 2
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 1.0 milliliters of butyl titanates are measured, butyl titanate are added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 18 milligram two is then weighed
Water sodium molybdate, then 36 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
It is added in 20 ml deionized waters and fully dissolving prepares the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 2, the liquid growth on graphite fibre
Titanium dioxide nanoplate thickness be 75~100nm, width be 700~1000nm.With the nano titania of single structure
Piece is compared, and titanium dioxide nanoplate/graphite fiber composite materials promote the separation in light induced electron and hole, is effectively increased pair
The utilization rate of sunshine.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 2,
Stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.With titanium dioxide nanoplate/graphite fibre composite wood
Material is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are under ultraviolet light, visible ray to methyl orange
Higher photocatalysis efficiency is respectively provided with, the utilization rate to sunshine is effectively increased.
Embodiment 3
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 1.5 milliliters of butyl titanates are measured, butyl titanate are added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 18 milligram two is then weighed
Water sodium molybdate, then 36 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
It is added in 20 ml deionized waters and fully dissolving prepares the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 3, the liquid growth on graphite fibre
Titanium dioxide nanoplate thickness be 150~200nm, width be 1200~1700nm.Received with the titanium dioxide of single structure
Rice piece is compared, and titanium dioxide nanoplate/graphite fiber composite materials promote the separation in light induced electron and hole, effectively increase
To the utilization rate of sunshine.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fibre composite wood made from above-described embodiment 3
Material, stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.It is compound with titanium dioxide nanoplate/graphite fibre
Material is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are under ultraviolet light, visible ray to methyl
Orange is respectively provided with higher photocatalysis efficiency, effectively increases the utilization rate to sunshine.
Embodiment 4
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 1.0 milliliters of butyl titanates are measured, butyl titanate are added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 6 milligram of two water is then weighed
Sodium molybdate, then 12 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
Dissolve into 20 ml deionized waters and fully and prepare the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 4, the liquid growth on graphite fibre
Titanium dioxide nanoplate thickness be 75~100nm, width be 700~1000nm.With the nano titania of single structure
Piece is compared, and titanium dioxide nanoplate/graphite fiber composite materials promote the separation in light induced electron and hole, is effectively increased pair
The utilization rate of sunshine.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 4,
Stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.With titanium dioxide nanoplate/graphite fibre composite wood
Material is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are under ultraviolet light, visible ray to methyl orange
Higher photocatalysis efficiency is respectively provided with, the utilization rate to sunshine is effectively increased.
Embodiment 5
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 1.0 milliliters of butyl titanates are measured, butyl titanate are added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 18 milligram two is then weighed
Water sodium molybdate, then 36 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
It is added in 20 ml deionized waters and fully dissolving prepares the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 5, the liquid growth on graphite fibre
Titanium dioxide nanoplate thickness be 75~100nm, width be 700~1000nm.With the nano titania of single structure
Piece is compared, and titanium dioxide nanoplate/graphite fiber composite materials promote the separation in light induced electron and hole, is effectively increased pair
The utilization rate of sunshine.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 5,
Stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.With titanium dioxide nanoplate/graphite fibre composite wood
Material is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are under ultraviolet light, visible ray to methyl orange
Higher photocatalysis efficiency is respectively provided with, the utilization rate to sunshine is effectively increased.
Embodiment 6
Step 1：The hydrochloric acid solution and 0.3 gram of graphite fibre for measuring 18 milliliters 5 moles every liter first are sufficiently mixed stirring 10
Minute, prepare the first mixed liquor.
Step 2：Then 1.0 milliliters of butyl titanates are measured, butyl titanate are added drop-wise in the first mixed liquor dropwise, subsequently
Solution is sufficiently mixed uniformly within 30 minutes by magnetic agitation, produce the second mixed liquor.
Step 3：Then the hydrofluoric acid that 0.35 milliliter of mass fraction is 47% is measured, the second mixed liquor is added dropwise in hydrofluoric acid
In, stir 5 minutes, produce the 3rd mixed liquor.
Step 4：3rd mixed liquor is placed into hydrothermal reaction kettle, is reacted 4 hours at 180 DEG C, prepares the 4th mixed liquor.
Step 5：Filter the 4th mixed liquor and obtain sediment, by obtained sediment with aqueous isopropanol (deionized water with
Isopropanol volume ratio is 2:1) it is cleaned by ultrasonic 3 minutes, is then cleaned, finally spent with 0.1 mole every liter of sodium hydroxide solution
Ion water washing.Dried 12 hours under conditions of 60 DEG C followed by by the sediment after washing, be made titanium dioxide nanoplate/
Graphite fiber composite materials.
Step 6：Then 50 milligrams of titanium dioxide nanoplate/graphite fiber composite materials are weighed, 42 milligram two is then weighed
Water sodium molybdate, then 84 milligrams of thiocarbamides are weighed, titanium dioxide nanoplate/graphite fiber composite materials, Sodium Molybdate Dihydrate, thiocarbamide are added
It is added in 20 ml deionized waters and fully dissolving prepares the 5th mixed liquor.
Step 7：5th mixed liquor is placed into hydrothermal reaction kettle, reacted 24 hours at 200 DEG C, the 6th is prepared and mixes
Liquid.
Step 8：Filter the 5th mixed liquor and obtain sediment, obtained sediment is washed with deionized, followed by general
Sediment after washing is dried 12 hours under conditions of 50 DEG C, is finally taken out the molybdenum sulfide nanometer sheet/titanium dioxide being made and is received
Rice piece/graphite fiber composite materials.
Titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 6, the liquid growth on graphite fibre
Titanium dioxide nanoplate thickness be 75~100nm, width be 700~1000nm.With the nano titania of single structure
Piece is compared, and titanium dioxide nanoplate/graphite fiber composite materials promote the separation in light induced electron and hole, is effectively increased pair
The utilization rate of sunshine.Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials made from above-described embodiment 6,
Stratiform molybdenum sulfide nanometer sheet is mutually grown in titanium dioxide nanoplate upper liquid.With titanium dioxide nanoplate/graphite fibre composite wood
Material is compared, and molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials are under ultraviolet light, visible ray to methyl orange
Higher photocatalysis efficiency is respectively provided with, the utilization rate to sunshine is effectively increased.
Obtained titanium dioxide nanoplate/graphite fiber composite materials are respectively in ultraviolet light in Fig. 3 comparing embodiments 3,5
The photocatalytic activity of methyl orange solution and the change of time are understood under irradiation, butyl titanate addition is 1.0 milliliters of time
Catalytic degradation efficiency is high.
Obtained molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fibre is combined in Fig. 4 comparing embodiments 4,5,6
Material under radiation of visible light to the photocatalytic activity of methyl orange solution and the change of time respectively in ultraviolet light with understanding, two water
Sodium molybdate, thiocarbamide addition are respectively 18 milligrams, 36 milligram hour photocatalytic degradation efficiencies height.
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials, it is characterised in that the molybdenum sulfide
In nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials the thickness of the titanium dioxide nanoplate of liquid growth be 75~
100nm, width is 700~1000nm, and molybdenum sulfide nanometer sheet is covered in titanium dioxide nanoplate surface in stratiform.
2. a kind of preparation method of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials, it is characterised in that
Comprise the following steps that：
Step 1：After a certain amount of graphite fibre, hydrochloric acid solution are mixed, a certain amount of metatitanic acid is added dropwise after ultrasonic reaction grinding
Butyl ester, hydrogen fluoride solution are sufficiently stirred for preparing the first reaction solution；
Step 2：First mixed liquor is placed in hydrothermal reaction kettle, fully product is filtered after reaction, cleaned, drying is prepared into two
TiOx nano piece/graphite fiber composite materials；
Step 3：Take a certain amount of titanium dioxide nanoplate/graphite fiber composite materials to add appropriate Sodium Molybdate Dihydrate and thiocarbamide, use
Deionized water is made into the second reaction solution；
Step 4：Second mixed liquor is placed in hydrothermal reaction kettle after fully reaction product filtered respectively, cleaned, drying is made
Molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials.
3. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that the concrete operations of described step 1 are to take 18 milliliters, 5 moles every liter of hydrochloric acid solution and 0.3 gram of graphite
Fiber is sufficiently mixed stirring 10 minutes, is added dropwise dropwise after butyl titanate, solution is sufficiently mixed within 30 minutes by magnetic agitation
It is even, stirred 5 minutes after adding dropwise the hydrofluoric acid that 0.35 milliliter of mass fraction is 47%, produce mixed liquor.
4. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that the addition of butyl titanate is 0.5~1.5 milliliter in described step 1, preferred butyl titanate plus
Enter amount for 1.0 milliliters.
5. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that the hydrothermal reaction condition of described step 2：180 DEG C of reaction temperature, the reaction time is 4 hours, described
The concrete operations of the cleaning process of step 2 are：With aqueous isopropanol, (deionized water is 2 with isopropanol volume ratio:1) it is cleaned by ultrasonic
3 minutes, then the sediment after washing is cleaned with 0.1 mole every liter of sodium hydroxide solution, obtained sediment is spent again
Neutrality is arrived in ion washing, and the drying process of described step 2 is：Taken out after being dried 12 hours under conditions of 60 DEG C.
6. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that in described step 3 titanium dioxide nanoplate/graphite fiber composite materials addition be 50 milligrams, go from
Sub- water addition is 20 milliliters.
7. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that Sodium Molybdate Dihydrate and the mass ratio that thiocarbamide is added are 1 in described step 3：2, Sodium Molybdate Dihydrate preferably
Quality is 6-42 milligrams, and most preferred Sodium Molybdate Dihydrate and thiocarbamide addition are respectively 18 milligrams and 36 milligrams.
8. the preparation side of molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fiber composite materials as claimed in claim 2
Method, it is characterised in that hydrothermal reaction condition in described step 4：200 DEG C of reaction temperature, in 24 hours reaction time, described is clear
Wash, drying process is：Cleaned with deionized water, the drying temperature is 50 DEG C, the drying time is 12 hours.
9. a kind of catalysis material, it is characterised in that the catalysis material includes graphite fibre matrix and positioned at graphite fibre
The titanium dioxide nanoplate of matrix surface and the molybdenum sulfide nanosheet photocatalytic material for loading to titanium dioxide nanoplate surface, institute
Catalysis material is stated for molybdenum sulfide nanometer sheet/titanium dioxide nanoplate/graphite fibre composite photocatalyst material.
10. molybdenum sulfide nanometer sheet/titanium dioxide that a kind of any one of claim 2 to 8 claim methods described is prepared
Application of the titanium nanometer sheet/graphite fiber composite materials in photocatalysis field.
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