CN106881136A - Metal phase molybdenum bisuphide/two dimension carbonitride catalysis material preparation method - Google Patents
Metal phase molybdenum bisuphide/two dimension carbonitride catalysis material preparation method Download PDFInfo
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- molybdenum bisuphide
- carbonitride
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- catalysis material
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- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 60
- 239000011733 molybdenum Substances 0.000 title claims abstract description 60
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 46
- 239000002184 metal Substances 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000006555 catalytic reaction Methods 0.000 title claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 24
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- GICWIDZXWJGTCI-UHFFFAOYSA-I molybdenum pentachloride Chemical compound Cl[Mo](Cl)(Cl)(Cl)Cl GICWIDZXWJGTCI-UHFFFAOYSA-I 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000003426 co-catalyst Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910052799 carbon Inorganic materials 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000001699 photocatalysis Effects 0.000 claims description 6
- 238000006303 photolysis reaction Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 238000000280 densification Methods 0.000 claims description 2
- 239000003599 detergent Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 claims description 2
- 230000001737 promoting effect Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 4
- 229910052757 nitrogen Inorganic materials 0.000 claims 2
- 230000003993 interaction Effects 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 24
- 239000011941 photocatalyst Substances 0.000 abstract description 20
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000001354 calcination Methods 0.000 description 13
- 238000010792 warming Methods 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 229920000877 Melamine resin Polymers 0.000 description 5
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000009777 vacuum freeze-drying Methods 0.000 description 3
- 229910017311 Mo—Mo Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000000833 X-ray absorption fine structure spectroscopy Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- -1 carbonitride Chemical compound 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002468 redox effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
Abstract
Composite photo-catalyst the invention discloses a kind of metal phase molybdenum bisuphide and two-dimentional carbonitride and preparation method thereof.The material is 1 by mass ratio：1000~5:1000 molybdenum bisuphide and carbonitride is composited, and wherein molybdenum bisuphide is metal 1T phases, and carbonitride possesses dimensional thinlayer structure.The material preparation method comprises the following steps：(1) dimensional thinlayer carbonitride, molybdenum pentachloride and thioacetamide are scattered in dimethylformamide (DMF) be stirred, ultrasonic disperse treatment；(2) mixed liquor that will be obtained is added to the treatment of autoclave high temperature；(3) material is washed for several times by ethanol, deionized water after processing；(4) material freeze is dried to obtain prepared photochemical catalyst after washing.Photochemical catalyst prepared by the present invention has good decomposition water H2-producing capacity under visible light, and need not add noble metal platinum as co-catalyst.Preparation process is simple, and energy consumption is low, low cost, easily realizes.
Description
Technical field
The present invention relates to catalysis material, a kind of metal phase (1T) molybdenum bisuphide/dimensional thinlayer carbonitride visible ray is refered in particular to
The preparation and use of composite photo-catalyst, belongs to composite and photodissociation aquatic products hydrogen technical field.
Background technology
From last century the seventies so far, the development problem of traditional energy shortage and new energy is constantly subjected to educational circles
With social extensive concern.Hydrogen Energy is possessed as replacement traditional energy as a kind of green energy resource that can be obtained by decomposition water
Potentiality.For a long time, the research of the light decomposition aquatic products hydrogen based on semiconductors such as titanium dioxide has obtained extraordinary development, but
Be conventional semiconductors light utilization ratio it is limited, catalyst quantum efficiency is relatively low, to the excessive need of co-catalyst noble metal platinum
The problems such as asking all limits the further development that light decomposes aquatic products hydrogen.
Carbonitride as a kind of new conductor photocatalysis material, because it possesses visible absorption ability, physico
Learn stable in properties and can under visible light illumination decompose aquatic products hydrogen, in recent years as a popular catalysis material.It passes through
The dimensional thinlayer carbonitride of square stripping method treatment is due to its larger specific surface area and redox property from top to bottom so that property
Can be further enhanced.Need to add noble metal platinum as co-catalyst to realize highly effective hydrogen yield in conventional photolytic aqueous systems,
Platinum expensive and earth storage level is limited, therefore explore the cheap stabilization photocatalytic water co-catalyst of substitution platinum and be also one and grind
The important directions studied carefully.The molybdenum bisuphide of metal phase (1T) not only possesses the electric conductivity and preferable stability of superelevation, and it is to hydrogen
The free energy of atomic adsorption is close to 0 so that it in theory can be as substitution platinum photodissociation aquatic products hydrogen co-catalyst.Therefore, originally
Invention provides a kind of preparation method of metal (1T) phase molybdenum bisuphide/dimensional thinlayer carbonitride visible light composite photocatalyst, should
Relative to single two-dimentional carbonitride, its visible photocatalysis water H2-producing capacity is significantly improved composite.
The content of the invention
It is an object of the invention to provide a kind of high-performance metal phase (1T) molybdenum bisuphide/bis- with low cost, stable in properties
The preparation method of thin layer carbonitride visible light composite photocatalyst is tieed up, monomer is effectively improved by the molybdenum bisuphide for loading a small amount of
The visible light catalytic of carbonitride produces hydrogen activity, realizes substitution of the cheap stabilization co-catalyst to noble metal platinum.
Realize that technical solution of the invention is：A kind of metal phase (1T) molybdenum bisuphide/dimensional thinlayer carbonitride is visible
Photoreactivation photochemical catalyst is 1 by mass ratio：1000~5:1000 molybdenum bisuphide and dimensional thinlayer carbonitride is composited, wherein
Molybdenum bisuphide is metal phase (1T), and carbonitride possesses dimensional thinlayer structure.The material preparation method comprises the following steps：
(1) dimensional thinlayer azotized carbon nano piece is obtained by the method for thermal oxide；The preparation scheme may be referred to
X.She,J.Wu,J.Zhong,H.Xu,Y.Yang,R.Vajtai,J.Lou,Y.Liu,D.Du,H.Li,P.M.Ajayan,
Oxygenated monolayer carbon nitride for excellent photocatalytic hydrogen
evolution and external quantum efficiency,Nano Energy,27(2016)138-146。
(2) successively by dimensional thinlayer carbonitride, molybdenum pentachloride, thioacetamide be added to stirring in dimethylformamide,
Ultrasonic disperse obtains mixed liquor.
(3) mixed liquor is transferred in autoclave, reactor is placed in the reaction of baking oven high temperature, is incited somebody to action after the completion of reaction
Matter detergent, the drying arrived, you can obtain described photochemical catalyst.
In step (1), described thermal oxidation process is that, with melamine as presoma, its addition is 2-10g in crucible
In, and first time calcining is carried out in Muffle furnace, melamine is polycondensed into body phase carbonitride；Subsequent body phase carbonitride is ground into
Powder, carbon dust is nitrogenized as presoma with the body phase of 100-800mg, and it is uniform to be tiled in porcelain boat, and two are carried out in Muffle furnace
Secondary calcining；Third firing is the product that porcelain boat is stayed in after dinectly bruning is calcined for second.
In step (1), in three calcination process the heating rate of Muffle furnace be respectively 2 DEG C/min, 5 DEG C/min,
2 DEG C/min, three times calcining keeping temperature is 550 DEG C, and soaking time is 4h, 1h, 1h.
In step (2), the volume mass ratio of dimethylformamide, carbonitride, thioacetamide and molybdenum pentachloride
For：30ml：100mg：2.25g：0.0003-0.017g.
In step (2), mixing time is 20-50min, and ultrasonic time is 30-60min.
In step (3), the heating-up temperature of baking oven is 150-220 DEG C, and the reaction time is 24h.
In step (3), washing is washed 3 times by ethanol, and deionized water is washed 3 times, subsequent freeze-drying
24h。
The present invention compared with prior art, its significant advantage：Using in-situ method by the metal phase (1T) of thermodynamics meta-stable
Molybdenum bisuphide original position is supported on dimensional thinlayer carbonitride, obtains metal phase molybdenum bisuphide/two dimension nitridation carbon composite, and
The metal phase molybdenum bisuphide and two carbonitrides for making thermodynamics meta-stable are closely combined together, and the interface for obtaining densification is mutual
Effect, enables the photoelectron on two carbonitrides smoothly to move on metal phase molybdenum bisuphide, reaches light induced electron and hole
Efficiently separate, so as to effective its promoting catalysis in photocatalysis hydrogen production, the in situ metal for loading on two carbonitrides
Phase molybdenum bisuphide can effectively replace noble metal platinum to do photolysis water hydrogen co-catalyst, realize catalyst under excited by visible light
Obtain the high activity of photodissociation aquatic products hydrogen.Next metal phase molybdenum bisuphide of the invention/two dimension carbonitride composite material and preparation method thereof
Simply, low cost, is conducive to industrialized development.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram that prepared metal phase molybdenum bisuphide/two dimension nitrogenizes carbon composite photocatalyst.
Fig. 2 is the transmission electron microscope picture that prepared metal phase molybdenum bisuphide/two dimension nitrogenizes carbon composite photocatalyst.
Fig. 3 is the X of prepared metal phase molybdenum bisuphide/two dimension nitridation carbon composite photocatalyst and semiconductor phase molybdenum bisuphide
Ray Absorption Fine Structure spectrum.
Fig. 4 is the X of prepared metal phase molybdenum bisuphide/two dimension nitridation carbon composite photocatalyst and semiconductor phase molybdenum bisuphide
Fourier's conversion of ray Absorption Fine Structure spectrum.
Fig. 5 is that prepared metal phase molybdenum bisuphide/two dimension decomposes aquatic products under nitrogenizing carbon composite photocatalyst radiation of visible light
Hydrogen performance test figure.
Specific embodiment
Make further details of elaboration to the present invention below in conjunction with the accompanying drawings.
Embodiment 1：The preparation of metal phase (1T) molybdenum bisuphide/dimensional thinlayer carbonitride visible light composite photocatalyst includes
Following steps：
(1) melamine is placed in ceramic crucible with cover, 550 DEG C is warming up to 2 DEG C/min speed in Muffle furnace
Calcining 4h, obtains yellow substance grind into powder, then by yellow powder 500mg be laid in Noah's ark in Muffle furnace with 5 DEG C/
The speed of min is warming up to 550 DEG C of calcining 1h, then is warming up to 550 DEG C of calcining 1h with the speed of 2 DEG C/min, obtains two-dimentional carbonitride.
(2) in 30ml dimethylformamides being added into beaker, then by 100mg carbonitrides, 0.0003g molybdenum pentachlorides, 2.25g
Thioacetamide is added thereto stirring 30min, ultrasound 30min dispersions.
(3) mixed liquor is transferred in autoclave, reactor is placed in 200 DEG C of reaction 24h in baking oven, after the completion of reaction
Obtain substance migration ethanol, deionized water washing and vacuum freeze drying, you can obtain 0.1wt% metal phases (1T) curing
Molybdenum/two dimension nitrogenizes carbon composite photocatalyst (0.0001/0.1=0.1wt%).
Embodiment 2：The preparation of metal phase (1T) molybdenum bisuphide/two dimension carbonitride visible light composite photocatalyst includes following
Step：
(1) melamine is placed in ceramic crucible with cover, 550 DEG C is warming up to 2 DEG C/min speed in Muffle furnace
Calcining 4h, obtains yellow substance grind into powder, then by yellow powder 400mg be laid in Noah's ark in Muffle furnace with 5 DEG C/
The speed of min is warming up to 550 DEG C of calcining 1h, then is warming up to 550 DEG C of calcining 1h with the speed of 2 DEG C/min, obtains two-dimentional carbonitride.
(2) in 30ml dimethylformamides being added into beaker, then by 100mg carbonitrides, 0.0007g molybdenum pentachlorides, 2.25g
Thioacetamide is added thereto stirring 30min, ultrasound 30min dispersions.
(3) mixed liquor is transferred in autoclave, reactor is placed in 200 DEG C of reaction 24h in baking oven, after the completion of reaction
Obtain substance migration ethanol, deionized water washing and vacuum freeze drying, you can obtain 0.2wt% metal phases (1T) curing
Molybdenum/two dimension nitrogenizes carbon composite photocatalyst (0.0002/0.1=0.2wt%).
Embodiment 3：The preparation of metal phase (1T) molybdenum bisuphide/two dimension carbonitride visible light composite photocatalyst includes following
Step：
(1) melamine is placed in ceramic crucible with cover, 550 DEG C is warming up to 2 DEG C/min speed in Muffle furnace
Calcining 4h, obtains yellow substance grind into powder, then by yellow powder 500mg be laid in Noah's ark in Muffle furnace with 5 DEG C/
The speed of min is warming up to 550 DEG C of calcining 1h, then is warming up to 550 DEG C of calcining 1h with the speed of 2 DEG C/min, obtains two-dimentional carbonitride.
(2) in 30ml dimethylformamides being added into beaker, then by 100mg carbonitrides, 0.0017g molybdenum pentachlorides, 2.25g
Thioacetamide is added thereto stirring 30min, ultrasound 30min dispersions.
(3) mixed liquor is transferred in autoclave, reactor is placed in 200 DEG C of reaction 24h in baking oven, after the completion of reaction
Obtain substance migration ethanol, deionized water washing and vacuum freeze drying, you can obtain 0.5wt% metal phases (1T) curing
Molybdenum/two dimension nitrogenizes carbon composite photocatalyst (0.0005/0.1=0.5wt%).
Fig. 1 is the X-ray diffractogram that prepared metal phase molybdenum bisuphide/dimensional thinlayer nitrogenizes carbon composite photocatalyst, way
Middle diffraction maximum matches with carbonitride, because molybdenum disulfide content is less, so its XRD diffraction maximum is not able to observe that.
Fig. 2 is the transmission electron microscope picture that prepared metal phase molybdenum bisuphide/dimensional thinlayer nitrogenizes carbon composite photocatalyst.From figure
In it can be seen that two-dimentional carbonitride in class Graphene superthin structure, two dimension nitridation supported on carbon surface has molybdenum bisuphide.
Fig. 3 is prepared metal phase molybdenum bisuphide/dimensional thinlayer nitridation carbon composite photocatalyst and semiconductor phase curing
The X-ray absorption fine structure spectroscopy of molybdenum.As can be seen from the figure prepared metal phase molybdenum bisuphide and the sulphur of semiconductor phase two
Change molybdenum and visibly different curve is presented, illustrate that prepared molybdenum bisuphide interior atoms are arranged relative to semiconductor phase molybdenum bisuphide
Have occurred and that change.
Fig. 4 is prepared metal phase molybdenum bisuphide/dimensional thinlayer nitridation carbon composite photocatalyst and semiconductor phase curing
Fourier's conversion of the X-ray absorption fine structure spectroscopy of molybdenum.In figure it can be seen that Mo-Mo keys peak skew, Mo-Mo keys with
The reduction of Mo-S key peak intensities, molybdenum bisuphide is in metal phase in illustrating prepared catalyst.
Fig. 5 is decomposition under prepared metal phase molybdenum bisuphide/dimensional thinlayer nitridation carbon composite photocatalyst radiation of visible light
Aquatic products hydrogen performance test figure.It can be seen that two dimension nitridation carbon monomer H2-producing capacity is relatively low in figure, success gold-supported symbolic animal of the birth year curing
After molybdenum, H2-producing capacity is substantially improved, wherein the H2-producing capacity of 0.2% load capacity is preferably, 5h light-catalyzed reaction hydrogen outputs reach
9208mol/g。
Claims (8)
1. metal phase molybdenum bisuphide/two dimension carbonitride catalysis material, it is characterised in that：The catalysis material is by mass ratio
1：1000~5:1000 molybdenum bisuphide and dimensional thinlayer carbonitride is composited, and wherein molybdenum bisuphide is metal phase (1T), nitrogen
Change carbon and possess dimensional thinlayer structure；The metal phase molybdenum bisuphide of thermodynamics meta-stable and two carbonitrides are closely combined one
Rise, obtain the interfacial interaction of densification, the photoelectron on two carbonitrides is smoothly moved to metal phase molybdenum bisuphide
On, efficiently separating for light induced electron and hole is reached, so as to effective its promoting catalysis in photocatalysis hydrogen production, in two nitrogen
The metal phase molybdenum bisuphide for changing load in situ on carbon can effectively replace noble metal platinum to do photolysis water hydrogen co-catalyst, realize
Catalyst obtains the high activity of photodissociation aquatic products hydrogen under excited by visible light.
2. metal phase molybdenum bisuphide as claimed in claim 1/two dimension carbonitride catalysis material, it is characterised in that：The light
Catalysis material is 2 by mass ratio:1000 molybdenum bisuphide and dimensional thinlayer carbonitride is composited.
3. the preparation method of metal phase molybdenum bisuphide as claimed in claim 1/two dimension carbonitride catalysis material, its feature exists
In：Dimensional thinlayer carbonitride, molybdenum pentachloride, thioacetamide are added to stirring, ultrasonic disperse in dimethylformamide successively
Obtain mixed liquor；Mixed liquor is transferred in autoclave, reactor is placed in the reaction of baking oven high temperature, is incited somebody to action after the completion of reaction
Matter detergent, the drying arrived, you can obtain described catalysis material.
4. the preparation method of metal phase molybdenum bisuphide as claimed in claim 3/two dimension carbonitride catalysis material, its feature exists
In：The volume mass ratio of dimethylformamide, dimensional thinlayer carbonitride, thioacetamide and molybdenum pentachloride is：30ml：100mg：
2.25g：0.0003-0.017g.
5. the preparation method of the metal phase molybdenum bisuphide as described in claim 3 or 4/two dimension carbonitride catalysis material, it is special
Levy and be：The volume mass ratio of dimethylformamide, dimensional thinlayer carbonitride, thioacetamide and molybdenum pentachloride is：30ml：
100mg：2.25g：0.0007g.
6. the preparation method of metal phase molybdenum bisuphide as claimed in claim 3/two dimension carbonitride catalysis material, its feature exists
In：Mixing time is 20-50min, and ultrasonic time is 30-60min.
7. the preparation method of metal phase molybdenum bisuphide as claimed in claim 3/two dimension carbonitride catalysis material, its feature exists
In：The heating-up temperature of baking oven is 150-220 DEG C, and the reaction time is 24h.
8. the preparation method of metal phase molybdenum bisuphide as claimed in claim 3/two dimension carbonitride catalysis material, its feature exists
In：Washing is washed 3 times by ethanol, and deionized water is washed 3 times, subsequent freeze-drying 24h.
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| CN107829106A (en) * | 2017-11-01 | 2018-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of molybdenum sulfide/nitridation carbon composite and products thereof and application |
| CN107930665A (en) * | 2017-10-27 | 2018-04-20 | 浙江工商大学 | A kind of two dimension MoS2Photochemical catalyst of regulation and control and its preparation method and application |
| CN108404955A (en) * | 2018-01-16 | 2018-08-17 | 江苏大学 | Two selenizing molybdenum of metal phase/two dimension carbonitride catalysis material and preparation method |
| CN108467020A (en) * | 2018-05-24 | 2018-08-31 | 淮阴师范学院 | A kind of CN materials, preparation method and the purposes of high-specific surface area |
| CN108607581A (en) * | 2018-05-11 | 2018-10-02 | 湖北民族学院 | A kind of synthetic method of the molybdenum disulfide material with absorption-photocatalysis performance and application |
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| CN108889326A (en) * | 2018-07-02 | 2018-11-27 | 北京理工大学 | A kind of preparation method of molybdenum disulfide and the three-dimensional network frame of graphite phase carbon nitride |
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| CN114618556A (en) * | 2022-04-02 | 2022-06-14 | 中山大学 | Preparation of molybdenum disulfide composite carbon nitride material rich in sulfur vacancy and application of molybdenum disulfide composite carbon nitride material in aspect of photocatalytic hydrogen production |
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