CN109225276A - The flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind and synthetic method and application - Google Patents
The flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind and synthetic method and application Download PDFInfo
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 84
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 84
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 52
- 239000011733 molybdenum Substances 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 37
- -1 carbon nano tube compound Chemical class 0.000 title claims abstract description 32
- 238000010189 synthetic method Methods 0.000 title claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 230000001376 precipitating effect Effects 0.000 claims description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 8
- 230000001699 photocatalysis Effects 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000007146 photocatalysis Methods 0.000 claims description 7
- 229910015667 MoO4 Inorganic materials 0.000 claims description 6
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000011684 sodium molybdate Substances 0.000 claims description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000020477 pH reduction Effects 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 238000010129 solution processing Methods 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims 1
- 230000005494 condensation Effects 0.000 claims 1
- 238000006555 catalytic reaction Methods 0.000 abstract description 5
- 238000013461 design Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 235000016768 molybdenum Nutrition 0.000 description 41
- 230000005540 biological transmission Effects 0.000 description 6
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 241000165940 Houjia Species 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005406 washing Methods 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
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- 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
- B01J35/33—Electric or magnetic 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
- B01J35/30—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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/02—Preparation of oxygen
- C01B13/0203—Preparation of oxygen from inorganic compounds
- C01B13/0207—Water
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- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to catalysis material exploitation design and application fields, disclose the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind and its synthetic method and application.In flower-shaped two selenizings molybdenum/carbon nano tube compound material according to the present invention, the mass ratio of flower-shaped two selenizings molybdenum and carbon nanotube is 1:0.025-1.The carbon nanotube is uniformly adhered on flower-shaped two selenizings molybdenum.Preparation method are as follows: the present invention will be added in two selenizing molybdenum solutions to be synthesized containing carbon nanotube, in 180-240 DEG C of progress hydro-thermal reaction.Eccentric cleaning, dry, flower-shaped two selenizings molybdenum/carbon nano tube compound material under vacuum environment are carried out later.The method of the present invention is simple, reproducible, has a good application prospect.
Description
Technical field
The invention belongs to catalysis material exploitation design and application fields, are related to a kind of flower-shaped two selenizings molybdenum/carbon nanotube
Composite material and synthetic method and application.
Technical background
Two selenizing molybdenums the energy storage of Yin Qigao and good rub often by as a kind of lubricant and battery cathode material
Performance is wiped by extensive concern, while two selenizing molybdenums of floriform appearance have ultra-thin lamellar structure, there is biggish surface area, gather around
There are preferable absorbing properties.However there is serious defect, surfaces in electronic transmission process for pure flower-shaped two selenizings molybdenum
Product cannot be come into full contact with.Structure change of the two selenizing molybdenums in electronic transmission process can be enhanced by additional framework material,
Recent domestic scholar has studied more composite construction, but main concentrate is carbon material, including hollow carbon sphere, graphene
Deng.However as framework material, carbon nanotube has its unique structure, therefore carbon nanotube combines not with flower-shaped two selenizings molybdenum
Losing is a kind of optimization approach.But up to the present, it is not used as in photocatalysis about carbon nanotube and flower-shaped two selenizings molybdenum also
Research in terms of co-catalyst.
Summary of the invention
The present invention provides a kind of flower-shaped two selenizings molybdenum/carbon nano tube compound materials and its preparation method and application.
The first purpose of this invention is to introduce a kind of flower-shaped two selenizings molybdenum/carbon nano tube compound material.
The flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind is that carbon nanotube is uniformly adhered to flower-shaped two selenizings molybdenum
On, when this sandwich is used for photocatalysis, the feature that flower-shaped two selenizings molybdenum surface area can be made full use of big, raising can
Light-exposed absorptivity, moreover it is possible to using the good electric conductivity of carbon nanotube, promote the light induced electron generated in photocatalytic process
With the separation in hole, photocatalysis efficiency is improved；Therefore, this sandwich can significantly improve visible light to organic pollutant
Degradation efficiency, improve visible light photodissociation aquatic products oxygen efficiency, and improve solar energy electrotransformation efficiency etc..
The mass ratio of a kind of flower-shaped two selenizings molybdenum/carbon nano tube compound material, flower-shaped two selenizings molybdenum and carbon nanotube is 1:
0.025-0.1, the carbon nanotube are uniformly attached to the surface of flower-shaped two selenizings molybdenum.
Further, flower-shaped two selenizings molybdenum and the mass ratio of carbon nanotube are 1:0.075.
A kind of synthetic method of flower-shaped two selenizings molybdenum/carbon nano tube compound material, steps are as follows:
1) carbon nanotube is subjected to acidification:
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, hydro-thermal reaction is carried out, collects precipitating after reaction, is added third
Ketone solution, is cleaned by ultrasonic, and precipitating is collected, and is cleaned for several times with deionized water and alcohol, drying；Grinding, it is spare；
2) the complete carbon nanotube of step (1) acidification is added in reaction kettle, Na is added later2MoO4·2H2O, Se
Powder and NaBH4And ethanol water, mixed solution is obtained, vacuum oven heat preservation is put into, after heat preservation, collects precipitating,
Then precipitating is placed in NaOH solution processing, finally carries out eccentric cleaning, vacuum drying.
In step (1), the proportion of carbon nanotube and concentrated nitric acid is (20-80mg): (50-100mL).
In step (1), the temperature of hydro-thermal reaction is 80-150 DEG C, and the time is 1 hour；Ultrasonic time is 30-60min.
In step (2), in the mixed solution, carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration difference
For 0.5-2g/L, 0.1-0.16mol/L, 0.4-0.5mol/L, 0.15-0.18mol/L；In ethanol water, alcohol: the body of water
Product is than being 1:1.
In step (2), in vacuum oven, holding temperature is 180-240 DEG C, and the time is for 24 hours.
In step (2), the condition that is handled in NaOH solution are as follows: described with processing 2-6 hours under the conditions of 60-80 DEG C
NaOH solution concentration is 8-10mol/L.
The flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind prepared by the present invention is applied to photocatalysis Decomposition aquatic products oxygen
Purposes.
The invention has the benefit that
(1) the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind prepared by the present invention, carbon nanotube can be equably
It is attached on flower-shaped two selenizings molybdenum.
(2) the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind prepared by the present invention both can be in light-catalyzed reaction
The contact surface area of two selenizing molybdenums is improved, and electron hole can be promoted to separate.
(3) a kind of flower-shaped two selenizings molybdenum/carbon nano tube compound material can be applied to the co-catalyst in photocatalysis.
Detailed description of the invention
Fig. 1 is the scanning electron microscope on flower-shaped two selenizings molybdenum/carbon nano tube compound material surface obtained by the embodiment of the present invention 1
Photo.
Fig. 2 is the transmission results of flower-shaped two selenizings molybdenum/carbon nano tube compound material obtained by the embodiment of the present invention 1.
Fig. 3 is the scanning electron microscope on flower-shaped two selenizings molybdenum/carbon nano tube compound material surface obtained by the embodiment of the present invention 2
Photo.
Fig. 4 is the production oxygen of flower-shaped two selenizings molybdenum/carbon nano tube compound material and silver orthophosphate obtained by the embodiment of the present invention 3
Effect picture.
Specific implementation step
Below in conjunction with drawings and examples, the present invention is described in further detail.
Embodiment 1
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, wherein carbon nanotube and the proportion of concentrated nitric acid are 20mg:
100ml；Hydrothermal temperature is 100 DEG C, and heating time is 1 hour；Precipitating is collected after reaction, and acetone soln is added, is surpassed
Sound, time 30min；Cleaning 3 times is carried out with deionized water and alcohol later；Drying；Grinding, it is spare；
The carbon nanotube that above step has been handled is added in reaction kettle, and Na is added later2MoO4·2H2O, Se powder and
NaBH4 and ethanol water, wherein carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration be respectively 0.5g/L,
0.14mol/L, 0.49mol/L, 0.17mol/L.Wherein ethanol water is 40ml (alcohol: water=1:1)；It is put into vacuum drying
Case, holding temperature are 220 DEG C, and the time is for 24 hours；Precipitating is collected, is handled 2 hours under the conditions of 80 DEG C with NaOH solution, NaOH is molten
Liquid concentration is 10mol/L；Eccentric cleaning is finally carried out, dries, obtains sample 1.
As depicted in figs. 1 and 2, Fig. 1 can be seen that for the transmission and scanning of the composite material of carbon nanotube and two selenizing molybdenums
There is a small amount of carbon nanotube on two flower-shaped selenizing molybdenums, this is because content of carbon nanotubes in the composite is lower and carbon
Nanometer pipe size it is smaller, from low power lens under be not readily observed.It is clear that composite material has flower under Fig. 2 high power lens
Two selenizing molybdenum of shape and carbon nanotube composition, network-like carbon nanotube are effectively combined with flower-shaped two selenizings molybdenum, not only improve light
The absorption of visible light in catalysis, and be conducive to the transmission of electronics, and also further demonstrate carbon nanotube and two selenizing molybdenums
The successful synthesis of composite material.
Embodiment 2:
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, wherein carbon nanotube and the proportion of concentrated nitric acid are 80mg:
100ml；Hydrothermal temperature is 120 DEG C, and heating time is 1 hour；Precipitating is collected after reaction, and acetone soln is added, is surpassed
Sound, time 60min；Cleaning 3 times is carried out with deionized water and alcohol later；Drying；Grinding, it is spare；
The carbon nanotube that above step has been handled is added in reaction kettle, and Na is added later2MoO4·2H2O, Se powder and
NaBH4And ethanol water, wherein carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration be respectively 2g/L,
0.14mol/L, 0.45mol/L, 0.15mol/L.Wherein ethanol water is 50ml (alcohol: water=1:1)；It is put into vacuum drying
Case, holding temperature are 220 DEG C, and the time is for 24 hours；Precipitating is collected, is handled 6 hours under the conditions of 80 DEG C with NaOH solution, NaOH is molten
Liquid concentration is 10mol/L；Eccentric cleaning is finally carried out, dries, obtains sample 2.
Carbon nanotube and composite material (Fig. 3) scanning figure of two selenizing molybdenums can be seen that when content of carbon nanotubes is higher,
Carbon nanotube is uniformly wrapped on flower-shaped two selenizings molybdenum, and the carbon nanotube covered on flower-shaped two selenizings molybdenum surface is more conducive to
The transmission of electronics carries out light-catalyzed reaction more efficiently.
Embodiment 3
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, wherein carbon nanotube and the proportion of concentrated nitric acid are 20mg:
100ml；Hydrothermal temperature is 80 DEG C, and heating time is 1 hour；Precipitating is collected after reaction, and acetone soln is added, is surpassed
Sound, time 30min；Cleaning 3 times is carried out with deionized water and alcohol later；Drying；Grinding, it is spare；
The carbon nanotube that above step has been handled is added in reaction kettle, and Na is added later2MoO4·2H2O, Se powder and
NaBH4 and ethanol water, wherein carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration be respectively 0.5g/L,
0.14mol/L, 0.49mol/L, 0.17mol/L.Wherein ethanol water is 40ml (alcohol: water=1:1)；It is put into vacuum drying
Case, holding temperature are 180 DEG C, and the time is for 24 hours；Precipitating is collected, is handled 2 hours under the conditions of 80 DEG C with NaOH solution, NaOH is molten
Liquid concentration is 10mol/L；Eccentric cleaning is finally carried out, dries, obtains sample 3.
Embodiment 4
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, wherein carbon nanotube and the proportion of concentrated nitric acid are 20mg:
100ml；Hydrothermal temperature is 150 DEG C, and heating time is 1 hour；Precipitating is collected after reaction, and acetone soln is added, is surpassed
Sound, time 30min；Cleaning 3 times is carried out with deionized water and alcohol later；Drying；Grinding, it is spare；
The carbon nanotube that above step has been handled is added in reaction kettle, and Na is added later2MoO4·2H2O, Se powder and
NaBH4 and ethanol water, wherein carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration be respectively 0.5g/L,
0.14mol/L, 0.49mol/L, 0.17mol/L.Wherein ethanol water is 40ml (alcohol: water=1:1)；It is put into vacuum drying
Case, holding temperature are 240 DEG C, and the time is for 24 hours；Precipitating is collected, is handled 2 hours under the conditions of 80 DEG C with NaOH solution, NaOH is molten
Liquid concentration is 10mol/L；Eccentric cleaning is finally carried out, dries, obtains sample 4.
Embodiment 5:
Flower-shaped two selenizings molybdenum/carbon nano tube compound material of 5mg is poured into 50ml deionized water, ultrasonic 3h, Zhi Houjia
Enter 0.3mol/L silver nitrate 30ML, dark reaction 12；0.1mol/L Na is added after reaction3PO4·12H2O solution 30ML；After
Continuous dark reaction 4h, centrifuge washing collect sample；Obtained above-mentioned sample 0.3g is weighed later, then takes 1gAgNO3As sacrificial
Domestic animal agent；It is dissolved in ultrasound 5min in 100ml water, it is therefore an objective to be uniformly mixed solution；It pours into the oxygen generating bottle produced in oxygen device, it is close
Seal oxygen generating bottle；It opens and produces oxygen mode, be protected from light 5 minutes, LED light is opened after 5min and irradiates the solution, with the growth of time,
It can be in the trend risen it can be seen that producing oxygen curve.Wherein pure phosphoric acid silver is as control.
From fig. 4, it can be seen that photocatalysis produces oxygen rate and rises rapidly, this is because silver orthophosphate and flower when LED light is opened
Two selenizing molybdenum of shape/carbon nano tube compound material has higher production oxygen activity under cooperating jointly, and after 10min, upper raising speed
Degree is slow, and the state that tends towards stability substantially, also illustrates that silver orthophosphate and flower-shaped two selenizings molybdenum/carbon nano tube compound material are stablized
Property it is high.And in 45min, silver orthophosphate and flower-shaped two selenizings molybdenum/carbon nano tube compound material produce oxygen rate and reach 23 μm of ol/L,
It is about 3 times that pure phosphoric acid silver produces oxygen rate, it is shown that silver orthophosphate and flower-shaped two selenizings molybdenum/carbon nano tube compound material are efficient
Production oxygen activity.
Claims (9)
1. a kind of flower-shaped two selenizings molybdenum/carbon nano tube compound material, it is characterised in that: in the composite material, flower-shaped two selenizing
Molybdenum and the mass ratio of carbon nanotube are 1:0.025-0.1, and the carbon nanotube is uniformly attached to the surface of flower-shaped two selenizings molybdenum.
2. the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind according to claim 1, it is characterised in that: described multiple
In condensation material, the mass ratio of flower-shaped two selenizings molybdenum and carbon nanotube is 1:0.075.
3. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 1, which is characterized in that
Steps are as follows:
1) carbon nanotube is subjected to acidification:
Carbon nanotube and concentrated nitric acid are poured into reaction kettle, hydro-thermal reaction is carried out, collects precipitating after reaction, it is molten that acetone is added
Liquid is cleaned by ultrasonic, and precipitating is collected, and is cleaned for several times with deionized water and alcohol, drying；Grinding, it is spare；
2) the complete carbon nanotube of step (1) acidification is added in reaction kettle, Na is added later2MoO4·2H2O, Se powder and
NaBH4And ethanol water, mixed solution is obtained, vacuum oven heat preservation is put into, after heat preservation, collects precipitating, then
Precipitating is placed in NaOH solution processing, finally carries out eccentric cleaning, vacuum drying.
4. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 3, which is characterized in that
In step (1), the proportion of carbon nanotube and concentrated nitric acid is (20-80mg): (50-100mL).
5. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 3, which is characterized in that
In step (1), the temperature of hydro-thermal reaction is 80-150 DEG C, and the time is 1 hour；Ultrasonic time is 30-60min.
6. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 3, which is characterized in that
In step (2), in the mixed solution, carbon nanotube, Na2MoO4·2H2O, Se powder and NaBH4Concentration be respectively 0.5-2g/
L, 0.1-0.16mol/L, 0.4-0.5mol/L, 0.15-0.18mol/L；In ethanol water, alcohol: the volume ratio of water is 1:
1。
7. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 3, which is characterized in that
In step (2), in vacuum oven, holding temperature is 180-240 DEG C, and the time is for 24 hours.
8. according to the synthetic method of the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in right 3, which is characterized in that
In step (2), the condition that is handled in NaOH solution are as follows: with processing 2-6 hours under the conditions of 60-80 DEG C, the NaOH solution is dense
Degree is 8-10mol/L.
9. the flower-shaped two selenizings molybdenum/carbon nano tube compound material of one kind described in claim 1 is used for photocatalysis Decomposition aquatic products oxygen
Purposes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777056A (en) * | 2020-07-13 | 2020-10-16 | 南昌航空大学 | Hydrated carbon/amorphous molybdenum selenide composite material and preparation method and application thereof |
| CN112321990A (en) * | 2020-11-11 | 2021-02-05 | 南开大学 | Preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material |
| CN112553651A (en) * | 2020-11-03 | 2021-03-26 | 常州大学 | Preparation method of selenide coated carbon nanotube material |
| CN113058603A (en) * | 2021-03-18 | 2021-07-02 | 内蒙古工业大学 | Two-dimensional fully-hydrolyzed carbon nanofiber material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007005038A1 (en) * | 2004-08-31 | 2007-01-11 | University Of Florida Research Foundation, Inc. | Photocatalytic nanocomposites and applications thereof |
| CN102992281A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
| KR20160132541A (en) * | 2015-05-11 | 2016-11-21 | 오원춘 | Photocatalyst for reduction and manufacturing method thereof |
| CN106521545A (en) * | 2016-10-10 | 2017-03-22 | 华南农业大学 | Preparing method for MoS2-CNT multi-level nano-structure electrolysis water hydrogen production material |
| CN107376948A (en) * | 2017-08-17 | 2017-11-24 | 哈尔滨工业大学 | A kind of preparation method of two-dimentional selenizing molybdenum functional material water electrolysis hydrogen production catalyst |
-
2018
- 2018-08-22 CN CN201810959553.8A patent/CN109225276B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007005038A1 (en) * | 2004-08-31 | 2007-01-11 | University Of Florida Research Foundation, Inc. | Photocatalytic nanocomposites and applications thereof |
| CN102992281A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
| KR20160132541A (en) * | 2015-05-11 | 2016-11-21 | 오원춘 | Photocatalyst for reduction and manufacturing method thereof |
| CN106521545A (en) * | 2016-10-10 | 2017-03-22 | 华南农业大学 | Preparing method for MoS2-CNT multi-level nano-structure electrolysis water hydrogen production material |
| CN107376948A (en) * | 2017-08-17 | 2017-11-24 | 哈尔滨工业大学 | A kind of preparation method of two-dimentional selenizing molybdenum functional material water electrolysis hydrogen production catalyst |
Non-Patent Citations (1)
| Title |
|---|
| YUNPENG HUANG ET AL.: "A CNT@MoSe2 hybrid catalyst for efficient and stable hydrogen evolution", 《NANOSCALE》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111777056A (en) * | 2020-07-13 | 2020-10-16 | 南昌航空大学 | Hydrated carbon/amorphous molybdenum selenide composite material and preparation method and application thereof |
| CN111777056B (en) * | 2020-07-13 | 2022-02-01 | 南昌航空大学 | Hydrated carbon/amorphous molybdenum selenide composite material and preparation method and application thereof |
| CN112553651A (en) * | 2020-11-03 | 2021-03-26 | 常州大学 | Preparation method of selenide coated carbon nanotube material |
| CN112321990A (en) * | 2020-11-11 | 2021-02-05 | 南开大学 | Preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material |
| CN112321990B (en) * | 2020-11-11 | 2022-07-12 | 南开大学 | Preparation method of molybdenum diselenide and carbon nano tube composite wave-absorbing material |
| CN113058603A (en) * | 2021-03-18 | 2021-07-02 | 内蒙古工业大学 | Two-dimensional fully-hydrolyzed carbon nanofiber material and preparation method thereof |
| CN113058603B (en) * | 2021-03-18 | 2023-01-10 | 内蒙古工业大学 | Two-dimensional fully-hydrolyzed carbon nanofiber material and preparation method thereof |
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