CN106914256A - The titania fiber and preparation method of load cadmium sulfide and molybdenum bisuphide - Google Patents
The titania fiber and preparation method of load cadmium sulfide and molybdenum bisuphide Download PDFInfo
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- CN106914256A CN106914256A CN201710108145.7A CN201710108145A CN106914256A CN 106914256 A CN106914256 A CN 106914256A CN 201710108145 A CN201710108145 A CN 201710108145A CN 106914256 A CN106914256 A CN 106914256A
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- cadmium sulfide
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- molybdenum bisuphide
- titania fiber
- loading
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 130
- 239000000835 fiber Substances 0.000 title claims abstract description 71
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 53
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 49
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 33
- 239000011733 molybdenum Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000011068 loading method Methods 0.000 claims abstract description 20
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 10
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 8
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 7
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 6
- 229940010552 ammonium molybdate Drugs 0.000 claims description 6
- 239000011609 ammonium molybdate Substances 0.000 claims description 6
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 6
- 235000018417 cysteine Nutrition 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 5
- 230000001788 irregular Effects 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 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 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 238000009987 spinning Methods 0.000 claims description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims 1
- PMUIBVMKQVKHBE-UHFFFAOYSA-N [S].NC(N)=O Chemical compound [S].NC(N)=O PMUIBVMKQVKHBE-UHFFFAOYSA-N 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 229910052982 molybdenum disulfide Inorganic materials 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002121 nanofiber Substances 0.000 abstract description 4
- 239000003403 water pollutant Substances 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 229910052961 molybdenite Inorganic materials 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000000975 dye Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000040710 Chela Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
Classifications
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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
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Optics & Photonics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of titania fiber and preparation method for loading cadmium sulfide and molybdenum bisuphide.First with high-voltage electrostatic spinning method, prepare fibrous titanium oxide fiber, then cadmium sulfide is loaded by hydro-thermal method, small-sized cadmium sulfide nanoparticles are formed in fiber surface, then flaky molybdenum disulfide is loaded again by hydro-thermal method, finally obtains the titanium dioxide nanofiber for having loaded cadmium sulfide and molybdenum bisuphide.The method of the present invention is simple, prepares product stable homogeneous, is easily separated and recovered from reaction system, and in photocatalytic degradation water pollutant, and hydrogen manufacturing, electro-catalysis, and sensor field has been applied.
Description
Technical field
The invention belongs to photocatalysis field, refer to load the preparation side of cadmium sulfide and molybdenum bisuphide titania fiber
Method.
Background technology
With the fast development of present industrial society, while material life is improved, environmental problem does not allow pleasure but
See.Treatment for discarding chemistry emission gets growing concern for.Waste water from dyestuff be main noxious industry waste water it
One.In numerous conductor photocatalysis materials, TiO2Because the advantages of high stability, nontoxic, non-secondary pollution and low cost,
Gas and the aspect such as water pollutant treatment and luminous energy conversion have very big application value.
But TiO2Have two it is clearly disadvantageous:One is greater band gap (anatase Eg=3.2eV), can only absorb λ<
The ultraviolet light of 387.5nm, sun light utilization efficiency is low；Two is that light induced electron is easily combined with hole.Solve these not enough, general meeting
By TiO2It is doped, area load semiconductor, dye sensitization or carried metal.
Synthesis TiO2Method have a lot, such as solid phase method, sol-gal process, hydro-thermal method, high-voltage electrostatic spinning method.Wherein,
Can easily synthesize continuous one-dimensional micro/nano-fibre using high-voltage electrostatic spinning method.Using one-dimensional titania fiber
As matrix, because its draw ratio is larger, relatively simple nano particle, it is easier to separated and recovered from reacted system,
So as to be used for multiple times.
Load method for semiconductor, generally there is infusion process, circumfluence method, physics (chemistry) vapour deposition process, hydro-thermal method etc..
Wherein hydro-thermal method refers in reactor, with water as medium, by heating, to form an environment for HTHP.By hydro-thermal
Method loads nano material, and relatively other methods are more environmentally friendly, and reaction condition is simply gentle, easily regulation and control, and product reunion is few, point
Dissipate property good.
The band gap of CdS semiconductor has photocatalytic in 2.4eV in visible-range.But cadmium sulfide compares table in itself
Area is small, easily by photoetch.The big titanium dioxide nanofiber of specific surface area is combined with cadmium sulfide, TiO is formed2/ CdS is combined
Structure has unique advantage, can efficiently separate electron hole pair.
MoS2It is class graphite ene-type, there is ultra-fine layer structure, band gap is in 1.89e V.The MoS of nanoscale2With than micron
Yardstick MoS2More excellent catalytic performance, in TiO2/ CdS area loads MoS2Nanometer sheet just can have a sample of synthesis
Larger adsorptivity and certain corrosion resistance, is conducive to the optimization of photochemical catalyst to use.
The present invention prepares titania fiber using high-pressure electrostatic method, recycles hydro-thermal method, and cysteine is used as vulcanizing agent
And chelating agent, in titania fiber area load cadmium sulfide.Similarly, make vulcanizing agent using thiocarbamide, born again in fiber surface
Molybdenum bisuphide is carried, has obtained loading the titania fiber of cadmium sulfide and molybdenum bisuphide.Current the method does not have been reported that.
The content of the invention
The present invention is the preparation method on load cadmium sulfide and molybdenum bisuphide titania fiber.The tri compound of synthesis
Catalyst TiO2/CdS/MoS2Light-catalysed light abstraction width, visible-range can be expanded to, meanwhile, the catalyst have than
Surface area is big, easily separated, recyclable, the advantages of photocatalysis efficiency is high.The catalyst cycle of synthesis is shorter, product stable homogeneous,
Degradable dyestuff type organic, with excellent photocatalytic activity.
The present invention prepares titania fiber using high-pressure electrostatic method, first with high-pressure electrostatic, precursor sol is stretched
Into threadiness, pure titania fiber is then obtained by sintering；Again by hydro-thermal method, cysteine is used as vulcanizing agent and chela
Close, in titania fiber area load cadmium sulfide.Similarly, make vulcanizing agent using thiocarbamide, two sulphur are loaded again in fiber surface
Change molybdenum, obtain loading the titania fiber of cadmium sulfide and molybdenum bisuphide.
Concretely comprise the following steps：
(1) by a certain amount of tetrabutyl titanate, acetylacetone,2,4-pentanedione, PVP, absolute ethyl alcohol after mixing a night, is obtained forerunner
Body colloidal sol, fiber membrane is obtained by electrostatic spinning machine；
(2) the fiber membrane low temperature drying for obtaining step (1), then 5 hours are incubated at 450 DEG C, obtain titanium dioxide fine
Dimension；
(3) product and cadmium nitrate that will be obtained by step (2), cysteine and pure water, mixing and stirring, are transferred to anti-
Answer in kettle, 12 hours are incubated at 120 DEG C, be then centrifuged for washing drying, obtain loading the titania fiber of cadmium sulfide；
(4) product and ammonium molybdate that will be obtained by step (3), thiocarbamide and pure water, mixing and stirring, are transferred to reactor
It is interior, 12 hours are incubated at 120 DEG C, drying is washed out, obtain loading the titania fiber of cadmium sulfide and molybdenum bisuphide.
3rd, the preparation method of a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide as claimed in claim 2, its
It is characterised by the precursor sol of electrostatic spinning, butyl titanate, acetylacetone,2,4-pentanedione, polyvinylpyrrolidone containing in ethanol
Amount is respectively 0.4g/mL, 0.2g/mL, 0.08g/mL.
4th, the preparation method of a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide as claimed in claim 2, its
Electrostatic spinning machine spinning is characterised by, shower nozzle tip is 15cm with the distance of receiver board, and voltage is 10 to 14k V.
5th, the preparation method of a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide as claimed in claim 2, its
When being characterized by hydro-thermal method load cadmium sulfide, content of the titania fiber in water is 5g/L, cadmium nitrate and half Guang ammonia
The molal quantity of acid is 1：3, the ratio between molal quantity of cadmium nitrate and titanium dioxide is less than 1.
6th, the preparation method of a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide as claimed in claim 2,
It is characterized in that using hydro-thermal method load molybdenum bisuphide when, load cadmium sulfide titania fiber in water content be 2.5g/
L, thiocarbamide is 2 with the mass ratio of ammonium molybdate：1, the ratio between molal quantity of ammonium molybdate and titanium dioxide is less than 1.
In the composite prepared, titania fiber irregular alignment, diameter is more than 1 in 200~500nm, length
Micron, there is fracture, and fiber surface has loaded granular cadmium sulfide, and outermost layer has loaded the molybdenum bisuphide of superfine sheet.
The load cadmium sulfide that the present invention is provided, the preparation characteristic of the titania fiber of molybdenum bisuphide is：
(1) step is simple and clear, and reactant is simple, reunites few, it is easy to control, titanium dioxide is prepared by method of electrostatic spinning
Nanofiber, then complete the compound of titania fiber and cadmium sulfide and molybdenum bisuphide by two one-step hydrothermals.And it is possible to control
Experiment parameter processed, adjusts the content of composite material surface loaded article.
(2) in the trielement composite material obtained by, titania fiber irregular alignment, fiber surface has loaded graininess
Cadmium sulfide, outermost layer loaded the molybdenum bisuphide of sheet.The composite of this structure and performance is easily from reaction system
Separation and recovery, in photocatalytic degradation water pollutant, and hydrogen manufacturing, electro-catalysis, and sensor field has been applied.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of product in embodiment 1, wherein, curve 1 represents pure titinium dioxide fiber, the generation of curve 2
Table has loaded the titania fiber of cadmium sulfide, and curve 3 represents the titania fiber for having loaded cadmium sulfide and molybdenum bisuphide；
Fig. 2 is the stereoscan photograph of pure titinium dioxide fiber in embodiment 1；
Fig. 3 is the stereoscan photograph of the titania fiber of area load cadmium sulfide in embodiment 1；
Fig. 4 is the stereoscan photograph of the titania fiber that cadmium sulfide and molybdenum sulfide have been loaded in embodiment 1；
Fig. 5 is the UV-vis DRS collection of illustrative plates of product in embodiment 1, and curve 1 represents pure titinium dioxide fiber, curve 2
Representative has loaded the titania fiber of cadmium sulfide, and curve 3 represents the titania fiber for having loaded cadmium sulfide and molybdenum bisuphide.
Below in conjunction with specific embodiment, further the present invention will be described.
Embodiment 1
The preparation method step of present embodiment is：
(1) by 4mL tetrabutyl titanates and 2mL acetylacetone,2,4-pentanediones, 0.8g PVP dissolve in 10mL absolute ethyl alcohols respectively, and stirring is equal
It is even, precursor sol is obtained；
(2) the appropriate colloidal sol that step (1) is obtained is injected in fluid Supplying apparatus (syringe), shower nozzle is sophisticated and receives
The distance of plate is 15cm, applies the voltage of 12k V, obtains fiber membrane；
(3) fiber membrane that step (2) is obtained is dried into 12h in a low temperature of less than 45 DEG C, then is placed on tube furnace
Interior, 1 DEG C/min heats up, and after taking-up in 5 hours is incubated at 450 DEG C, grinding obtains TiO2Fiber；
(4) titania fiber that step (3) is obtained is taken into 100mg, the cadmium nitrate with 77.5mg, the half Guang ammonia of 90mg
Acid, is dispersed in the pure water of 20mL, is transferred in the reactor of 30mL after stirring；
(5) in 120 DEG C of baking oven inside holding 12 hours, taking-up distilled water, ethanol washing, centrifugation, 60 DEG C of drying are obtained
Load the titania fiber of cadmium sulfide；
(6) titania fiber for having loaded cadmium sulfide that step (5) is obtained is taken into 50mg, with 20mg ammonium molybdates, 40mg
Thiocarbamide is dispersed in the pure water of 20mL, is transferred in the reactor of 30mL after stirring；
(7) in 120 degrees Celsius of baking oven inside holding 12 hours, taking-up distilled water, ethanol washing, centrifugation, 60 DEG C of drying,
Obtain loading the titania fiber of cadmium sulfide and molybdenum bisuphide.
Embodiment 2
The preparation method step of present embodiment is：
(1) by 4mL tetrabutyl titanates and 2mL acetylacetone,2,4-pentanediones, 0.8g PVP dissolve in 10mL absolute ethyl alcohols respectively, and stirring is equal
It is even, precursor sol is obtained；
(2) the appropriate colloidal sol that step (1) is obtained is injected in fluid Supplying apparatus (syringe), shower nozzle is sophisticated and receives
The distance of plate is 15cm, applies the voltage of 12k V, obtains fiber membrane；
(3) fiber membrane that step (2) is obtained is dried into 12h in a low temperature of less than 45 DEG C, then is placed on tube furnace
Interior, 1 DEG C/min heats up, and after taking-up in 5 hours is incubated at 450 DEG C, grinding obtains TiO2Fiber；
(4) titania fiber that step (3) is obtained is taken into 100mg, the cadmium nitrate with 62mg, the cysteine of 72mg,
It is dispersed in the pure water of 20mL, is transferred in the reactor of 30mL after stirring；
(5) in 120 degrees Celsius of baking oven inside holding 12 hours, taking-up distilled water, ethanol washing, centrifugation, 60 DEG C of drying,
Obtain loading the titania fiber of cadmium sulfide；
(6) titania fiber for having loaded cadmium sulfide that step (5) is obtained is taken into 50mg, with 25mg ammonium molybdates, 50mg
Thiocarbamide is dispersed in the pure water of 20mL, is transferred in the reactor of 30mL after stirring；
(7) in 120 degrees Celsius of baking oven inside holding 12 hours, taking-up distilled water, ethanol washing, centrifugation, 60 DEG C of drying,
Obtain loading the titania fiber of cadmium sulfide and molybdenum bisuphide.
Claims (6)
1. a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide, it is characterized by, titania fiber irregular alignment,
Diameter is more than 1 micron in 200~500nm, length, there is fracture, and fiber surface has loaded granular cadmium sulfide, outermost layer load
The molybdenum bisuphide of superfine sheet.
2. a kind of preparation method of the titania fiber of load cadmium sulfide and molybdenum bisuphide for described in claim 1 includes
Following steps：
(1) by a certain amount of tetrabutyl titanate, acetylacetone,2,4-pentanedione, PVP, absolute ethyl alcohol after mixing and stirring, is obtained presoma molten
Glue, fiber membrane is obtained by electrostatic spinning machine；
(2) the fiber membrane low temperature drying for obtaining step (1), then 5 hours are incubated at 450 DEG C, obtain titania fiber；
(3) product and cadmium nitrate that will be obtained by step (2), cysteine and pure water, mixing and stirring, are transferred to reactor
It is interior, 12 hours are incubated at 120 DEG C, it is then centrifuged for washing drying, obtain loading the titania fiber of cadmium sulfide；
(4) product and ammonium molybdate that will be obtained by step (3), thiocarbamide and pure water, mixing and stirring, are transferred in reactor,
12 hours are incubated at 120 DEG C, are then centrifuged for washing drying, obtain loading the titania fiber of cadmium sulfide and molybdenum bisuphide.
3. a kind of preparation method of the titania fiber for loading cadmium sulfide and molybdenum bisuphide, its feature as claimed in claim 2
Be electrostatic spinning precursor sol in, butyl titanate, acetylacetone,2,4-pentanedione, polyvinylpyrrolidone content in ethanol point
Wei not 0.4g/mL, 0.2g/mL, 0.08g/mL.
4. a kind of preparation method of the titania fiber for loading cadmium sulfide and molybdenum bisuphide, its feature as claimed in claim 2
It is electrostatic spinning machine spinning, shower nozzle tip is 15cm with the distance of receiver board, and voltage is 10~14kV.
5. a kind of preparation method of the titania fiber for loading cadmium sulfide and molybdenum bisuphide, its feature as claimed in claim 2
It is that when loading cadmium sulfide using hydro-thermal method, content of the titania fiber in water is 2~6g/L, cadmium nitrate and cysteine
Molal quantity be 1：3, the ratio between molal quantity of cadmium nitrate and titanium dioxide is less than 1.
6. the preparation method of a kind of titania fiber for loading cadmium sulfide and molybdenum bisuphide as claimed in claim 2, it is special
Levy be using hydro-thermal method load molybdenum bisuphide when, load cadmium sulfide titania fiber in water content be 2~6g/L, sulphur
Urea is 2 with the mass ratio of ammonium molybdate：1, the ratio between molal quantity of ammonium molybdate and titanium dioxide is less than 1.
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