CN108273540A - A kind of Mo doped graphites phase carbon nitride nanometer sheet powder and preparation method thereof - Google Patents
A kind of Mo doped graphites phase carbon nitride nanometer sheet powder and preparation method thereof Download PDFInfo
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- CN108273540A CN108273540A CN201810148642.4A CN201810148642A CN108273540A CN 108273540 A CN108273540 A CN 108273540A CN 201810148642 A CN201810148642 A CN 201810148642A CN 108273540 A CN108273540 A CN 108273540A
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- 239000000843 powder Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 47
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 46
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 26
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 24
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 24
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 41
- 229910021641 deionized water Inorganic materials 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 150000007974 melamines Chemical class 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 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
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005524 hole trap Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- -1 melamine Amine Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 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—
-
- B01J35/61—
-
- 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
-
- 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
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of preparation methods of Mo doped graphites phase carbon nitride nanometer sheet powder, make raw material with melamine, sodium molybdate, thiocarbamide and water, and modified presoma is prepared using sodium molybdate and thiocarbamide auxiliary hydro-thermal process melamine；Then high-temperature calcination is carried out to above-mentioned modified presoma, you can obtain Mo doping g C3N4Nanometer sheet powder.The invention also discloses the Mo being prepared using above method doping g C3N4Nanometer sheet powder.The Mo doping g C obtained3N4Nanometer powder is the nanometer sheet for having high-specific surface area, and metallic element Mo mixes g C3N4Band structure can be optimized in skeleton, be g C3N4The trap for providing more capture light induced electrons and hole, effectively increases the photocatalysis performance of material.The method of the present invention have the advantages that reaction process it is simple, it is easily controllable, low using cost of material, to equipment without particular/special requirement, be suitble to large-scale industrial production.
Description
Technical field
The invention belongs to catalysis material preparing technical fields, and in particular to a kind of Mo doped graphites phase carbon nitride nanometer sheet
The preparation method of powder further relates to the Mo doped graphite phase carbon nitride nanometer sheet powder being prepared using the above method.
Background technology
Clean energy resource and regenerative resource are the inevitable choices of human social development, to solve energy shortage and environmental degradation
Problem.Hydrogen has been acknowledged as optimal clean fuel, and combustion product is water, non-secondary pollution.g-C3N4Too as one kind
The semi-conducting material of sunlight response has received the extensive concern of people in photocatalysis field.Traditional body phase g-C3N4To purple
The absorption cut-off wave of outer visible light is about makes it have important application and commercial value in terms of photolysis water hydrogen in 460nm.
Document report：g-C3N4Photocatalysis performance and its electronic structure, specific surface area, microscopic appearance is directly related.And it passes
Body phase g-C prepared by system method3N4Specific surface area is small, is easily replied immediately soon to visible light-responded narrow range, light induced electron and hole
The low disadvantage of conjunction, photo-quantum efficiency seriously constrains the raising of its photocatalysis performance.Therefore, pass through g-C3N4It is modified to improve its light
The research of catalytic efficiency by people extensive favor.Conventional g-C3N4Modification strategies include mainly：Your gold Morphological control loads
Belong to, structure hetero-junctions and metal/non-metal adulterate.In particular, doping vario-property is primarily directed to g-C3N4Unique two-dimensional structure bone
Atom is replaced or is introduced between frame, optimizes photocatalytic by changing its electronic structure regulation and control valence band and conduction level position
Can, it is one of the maximally efficient method for realizing Energies control.In recent years, using metallic element (such as：Fe、Zn、K、Na、Cs、
Rb g-C) is adulterated3N4The document report for improving photocatalysis performance is subject to the people's attention, however, related Mo adulterates g- at present
C3N4The still rare document report of research, and photocatalysis performance enhancing mechanism be still not clear.
Therefore, the present invention provides a kind of modifies preparation Mo of forerunner to adulterate g-C3N4Strategy, first selection melamine,
Sodium molybdate, thiocarbamide and water make raw material, and modified melamine is prepared using sodium molybdate and thiocarbamide auxiliary hydro-thermal process melamine
Amine presoma；Then the melamine of above-mentioned modification is directly subjected to high-temperature calcination in air, you can obtain Mo and adulterate g-C3N4
Nanometer sheet powder.
Invention content
The object of the present invention is to provide a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder, solve existing
There is body phase g-C prepared by method3N4The easily quick disadvantage compound, photo-quantum efficiency is low of existing light induced electron and hole, in turn
The problem of constraining its photocatalysis performance.
It is a further object of the present invention to provide a kind of Mo doped graphites phase carbon nitride nanometer sheet powder.
The technical solution adopted in the present invention is a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder,
It is specifically implemented according to the following steps：
Step 1, the preparation of modified presoma：
Melamine, sodium molybdate, thiocarbamide, deionized water are added in reaction kettle, is stirred evenly, is put into baking oven and carries out water
Thermal response obtains solidliquid mixture；Then solidliquid mixture washed, dried, obtain modified presoma；
Step 2, Mo adulterates g-C3N4The preparation of nanometer sheet powder：
High-temperature calcination is carried out to the modification presoma that step 1 obtains and adulterates g-C to get to Mo3N4Nanometer sheet powder.
Feature of the present invention also resides in,
Melamine and the mass ratio of deionized water are 1 in step 1:60~1:2, the mass ratio of sodium molybdate and deionized water
It is 1:1000~1:100, the mass ratio of thiocarbamide and deionized water is 1:20~1:5.
Hydrothermal temperature is 120~200 DEG C in step 1, and the time is 12~96h.
It is washed in step 1, specially：Eccentric cleaning is distinguished 3~6 times using deionized water and absolute ethyl alcohol.
Drying temperature is 50~90 DEG C in step 1, and the time is 12~36h.
Step 2 high temperature calcination temperature is 500~600 DEG C, and soaking time is 1~6h.
Heating rate is 0.1~10 DEG C/min in calcination process.
The technical solution adopted in the present invention is a kind of Mo doped graphites phase carbon nitride nanometer sheet powder, using above-mentioned side
Method is prepared.
The invention has the advantages that
1, preparation method of the present invention have reaction process it is simple, it is easily controllable, low using cost of material, to equipment without special
It is required that the advantages of, the industrial scale applications of simple and environmentally-friendly low cost instantly have fully been catered to, large-scale industrial production is suitble to.Pass through
The dosage of melamine, thiocarbamide, sodium molybdate, deionized water is regulated and controled, the Mo with nanometer chip architecture can be prepared and mixed
Miscellaneous g-C3N4Nanometer powder.
2, the Mo doping g-C that the present invention is obtained3N4Nanometer powder is the nanometer sheet for having high-specific surface area, and metal is first
Plain Mo mixes g-C3N4Band structure can be optimized in skeleton, be g-C3N4Provide falling into for more capture light induced electrons and hole
Trap improves conventional bulk phase g-C3N4The quick compound defect of photo-generate electron-hole in semi-conducting material, to effectively increase
The photocatalysis performance of material.
Description of the drawings
Fig. 1 is Mo doping g-C prepared by the embodiment of the present invention 13N4The transmission electron micrograph of nanometer sheet powder；
Fig. 2 is Mo doping g-C prepared by the embodiment of the present invention 23N4The transmission electron micrograph of nanometer sheet powder.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder of the present invention, with melamine, sodium molybdate, sulphur
Urea and water make raw material, and modified cyanurotriamide presoma is prepared using sodium molybdate and thiocarbamide auxiliary hydro-thermal process melamine；
Then the melamine of above-mentioned modification is directly subjected to high-temperature calcination in air, you can obtain Mo and adulterate g-C3N4Nanometer sheet powder
End.
It is specifically implemented according to the following steps：
Step 1, the preparation of modified presoma：
Melamine is weighed, is put it into clean polytetrafluoroethyllining lining, sodium molybdate and thiocarbamide is added, after mixing,
The mass ratio of addition deionized water, melamine and deionized water is 1:60~1:2, the mass ratio of sodium molybdate and deionized water is
1:1000~1:100, thiocarbamide is 1 with deionized mass ratio:20~1:5, it is to be mixed uniform, it closes the lid and moves it into correspondence
Stainless steel cauldron housing, in an oven 120~200 DEG C heat preservation 12~96h, obtain presoma solidliquid mixture；It will be obtained
Presoma solidliquid mixture deionized water and absolute ethyl alcohol the difference eccentric cleaning obtained 3~6 times, what is obtained is deposited in 50~90
DEG C dry 12~36h, you can obtain modified melamine presoma.
Step 2, Mo adulterates g-C3N4The preparation of nanometer sheet powder：
The modified cyanurotriamide presoma that step 1 is obtained, is put into alumina crucible, closes the lid；Existed with Muffle furnace
Lower 500 DEG C~600 DEG C 1~6h of calcining of air atmosphere, calcining heating rate is 0.1~10 DEG C/min.It can be obtained Mo doping g-
C3N4Nanometer powder.
The present invention is using a kind of low cost, controllability and the good liquid and solid phase reaction method of operability and solid sintering technology phase
In conjunction with strategy, regulated and controled by the mass ratio to melamine, thiocarbamide, sodium molybdate, deionized water, can prepare has
The Mo of nanometer chip architecture adulterates g-C3N4Powder.
Mo produced by the present invention adulterates g-C3N4Nanometer powder has high specific surface area, and metallic element Mo mixes g-
C3N4Band structure can be optimized in skeleton, be g-C3N4The trap for providing more capture light induced electrons and hole, improves biography
Body phase of uniting g-C3N4The quick compound defect of photo-generate electron-hole in semi-conducting material, to improve the photocatalytic of material
Energy.O produced by the present invention adulterates g-C3N4Hydrogen-producing speed (870.6 μm of olg of nanometer sheet-1·h-1) more unmodified melamine
The body phase g-C that dinectly bruning is obtained3N4Hydrogen-producing speed (144.3 μm of olg-1·h-1) improve nearly 6.03 times.
And the method for the present invention have reaction process it is simple, it is easily controllable, low using cost of material, to equipment without particular/special requirement
The advantages of, the industrial scale applications of simple and environmentally-friendly low cost instantly have fully been catered to, large-scale industrial production is suitble to.
Embodiment 1
Step 1, it is 1 according to melamine and the mass ratio of deionized water:60, the mass ratio of sodium molybdate and deionized water is
1:1000, the mass ratio of thiocarbamide and deionized water is 1:5, melamine, sodium molybdate, thiocarbamide, deionized water are added clean
It mixes, stirs evenly in polytetrafluoroethyllining lining；Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is twisted
Tightly；It is put into baking oven, 12h, after furnace cooling, the solidliquid mixture that will be obtained, with deionized water and absolute ethyl alcohol are kept the temperature at 200 DEG C
Eccentric cleaning 6 times respectively, then, the dry 36h in 50 DEG C of baking ovens, you can obtain modified presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid；In 600 DEG C of isothermal holdings
2h, calcining heating rate are 0.1 DEG C/min, you can obtain Mo and adulterate g-C3N4Powder.
The Mo that the present embodiment obtains adulterates g-C3N4Powder TEM photos, as shown in Figure 1, it can be seen that it is apparent nanometer
Chip architecture.
Embodiment 2
Step 1, it is 1 according to melamine and the mass ratio of deionized water:2, the mass ratio of sodium molybdate and deionized water is
1:100, the mass ratio of thiocarbamide and deionized water is 1:20, melamine, sodium molybdate, thiocarbamide, deionized water are added clean
It mixes, stirs evenly in polytetrafluoroethyllining lining；Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is twisted
Tightly；It is put into baking oven, is kept the temperature at 180 DEG C for 24 hours, after furnace cooling, the solidliquid mixture that will be obtained, with deionized water and absolute ethyl alcohol
Distinguish eccentric cleaning 3 times, then, is dried in 60 DEG C of baking ovens for 24 hours, you can obtain modified presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid；In 550 DEG C of isothermal holdings
4h, calcining heating rate are 10 DEG C/min, you can obtain Mo and adulterate g-C3N4Powder.
The Mo that the present embodiment obtains adulterates g-C3N4Powder TEM photos, as shown in Figure 2, it can be seen that it is apparent nanometer
Chip architecture.
Embodiment 3
Step 1, it is 1 according to melamine and the mass ratio of deionized water:1, the mass ratio of sodium molybdate and deionized water is
1:500, the mass ratio of thiocarbamide and deionized water is 1:10, melamine, sodium molybdate, thiocarbamide, deionized water are added clean
It mixes, stirs evenly in polytetrafluoroethyllining lining；Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is twisted
Tightly；It is put into baking oven, 48h, after furnace cooling, the solidliquid mixture that will be obtained, with deionized water and absolute ethyl alcohol are kept the temperature at 160 DEG C
Eccentric cleaning 4 times respectively, then, the dry 12h in 90 DEG C of baking ovens, you can obtain modified presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid；In 500 DEG C of isothermal holdings
6h, calcining heating rate are 5 DEG C/min, you can obtain Mo and adulterate g-C3N4Powder.
Embodiment 4
Step 1, it is 1 according to melamine and the mass ratio of deionized water:30, the mass ratio of sodium molybdate and deionized water is
1:300, the mass ratio of thiocarbamide and deionized water is 1:15, melamine, sodium molybdate, thiocarbamide, deionized water are added clean
It mixes, stirs evenly in polytetrafluoroethyllining lining；Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is twisted
Tightly；It is put into baking oven, 72h, after furnace cooling, the solidliquid mixture that will be obtained, with deionized water and absolute ethyl alcohol are kept the temperature at 140 DEG C
Eccentric cleaning 5 times respectively, then, the dry 18h in 70 DEG C of baking ovens, you can obtain modified presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid；In 530 DEG C of isothermal holdings
4h, calcining heating rate are 8 DEG C/min, you can obtain Mo and adulterate g-C3N4Powder.
Embodiment 5
Step 1, it is 1 according to melamine and the mass ratio of deionized water:10, the mass ratio of sodium molybdate and deionized water is
1:800, the mass ratio of thiocarbamide and deionized water is 1:10, melamine, sodium molybdate, thiocarbamide, deionized water are added clean
It mixes, stirs evenly in polytetrafluoroethyllining lining；Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is twisted
Tightly；It is put into baking oven, 96h, after furnace cooling, the solidliquid mixture that will be obtained, with deionized water and absolute ethyl alcohol are kept the temperature at 120 DEG C
Eccentric cleaning 3 times respectively, then, the dry 30h in 80 DEG C of baking ovens, you can obtain modified presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid；In 570 DEG C of isothermal holdings
1h, calcining heating rate are 3 DEG C/min, you can obtain Mo and adulterate g-C3N4Powder.
Claims (8)
1. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder, which is characterized in that specifically according to the following steps
Implement：
Step 1, the preparation of modified presoma：
Melamine, sodium molybdate, thiocarbamide, deionized water are added in reaction kettle, stirred evenly, it is anti-to be put into progress hydro-thermal in baking oven
It answers, obtains solidliquid mixture；Then solidliquid mixture washed, dried, obtain modified presoma；
Step 2, Mo adulterates g-C3N4The preparation of nanometer sheet powder：
High-temperature calcination is carried out to the modification presoma that step 1 obtains and adulterates g-C to get to Mo3N4Nanometer sheet powder.
2. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In melamine and the mass ratio of deionized water are 1 in the step 1:60~1:2, the mass ratio of sodium molybdate and deionized water
It is 1:1000~1:100, the mass ratio of thiocarbamide and deionized water is 1:20~1:5.
3. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In hydrothermal temperature is 120~200 DEG C in the step 1, and the time is 12~96h.
4. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In being washed in the step 1, specially：Eccentric cleaning is distinguished 3~6 times using deionized water and absolute ethyl alcohol.
5. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In drying temperature is 50~90 DEG C in the step 1, and the time is 12~36h.
6. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In the step 2 high temperature calcination temperature is 500~600 DEG C, and soaking time is 1~6h.
7. a kind of preparation method of Mo doped graphites phase carbon nitride nanometer sheet powder according to claim 1 or 6, feature
It is, heating rate is 0.1~10 DEG C/min in the calcination process.
8. a kind of Mo doped graphites phase carbon nitride nanometer sheet powder, which is characterized in that using any one of the claim 1-7 sides
Method is prepared.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110302824A (en) * | 2019-08-06 | 2019-10-08 | 辽宁大学 | Molybdenum doping graphite phase carbon nitride catalyst and its preparation method and application |
| CN111013630A (en) * | 2019-12-23 | 2020-04-17 | 华北电力大学 | Heptamolybdate intercalated porous carbon nitride and preparation method and application thereof |
| CN111203262A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for rapidly preparing carbon nitride nanosheet loaded nano-copper, product and application thereof |
| CN113751048A (en) * | 2021-10-15 | 2021-12-07 | 阜阳师范大学 | Molybdenum trioxide in-situ intercalation carbon nitride composite catalyst and preparation method thereof |
| CN113769772A (en) * | 2021-09-01 | 2021-12-10 | 辽宁大学 | Hydrochloric acid treated Nb-Mo co-doped g-C3N4Photocatalytic material and preparation method and application thereof |
| CN115888788A (en) * | 2022-11-03 | 2023-04-04 | 常州大学 | Preparation method of three-dimensional honeycomb graphite phase carbon nitride composite photo-thermal catalyst, product and application thereof |
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| CN110026220B (en) * | 2019-04-22 | 2022-04-26 | 武汉科技大学 | Transition metal carbide/graphitized carbon-like composite powder and preparation method thereof |
| CN110026219A (en) * | 2019-04-22 | 2019-07-19 | 武汉科技大学 | A kind of transient metal doped g-C3N4Powder and preparation method thereof |
| CN110026220A (en) * | 2019-04-22 | 2019-07-19 | 武汉科技大学 | A kind of transition metal carbide/class graphitized carbon composite granule and preparation method thereof |
| CN110026219B (en) * | 2019-04-22 | 2022-04-29 | 武汉科技大学 | Transition metal doped g-C3N4Powder and preparation method thereof |
| CN110302824A (en) * | 2019-08-06 | 2019-10-08 | 辽宁大学 | Molybdenum doping graphite phase carbon nitride catalyst and its preparation method and application |
| CN110302824B (en) * | 2019-08-06 | 2021-10-22 | 辽宁大学 | Molybdenum-doped graphite-phase carbon nitride catalyst and preparation method and application thereof |
| CN111013630A (en) * | 2019-12-23 | 2020-04-17 | 华北电力大学 | Heptamolybdate intercalated porous carbon nitride and preparation method and application thereof |
| CN111013630B (en) * | 2019-12-23 | 2022-01-25 | 华北电力大学 | Heptamolybdate intercalated porous carbon nitride and preparation method and application thereof |
| CN111203262A (en) * | 2020-03-05 | 2020-05-29 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for rapidly preparing carbon nitride nanosheet loaded nano-copper, product and application thereof |
| CN111203262B (en) * | 2020-03-05 | 2023-03-31 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for rapidly preparing carbon nitride nanosheet loaded nano-copper, product and application thereof |
| CN113769772A (en) * | 2021-09-01 | 2021-12-10 | 辽宁大学 | Hydrochloric acid treated Nb-Mo co-doped g-C3N4Photocatalytic material and preparation method and application thereof |
| CN113751048A (en) * | 2021-10-15 | 2021-12-07 | 阜阳师范大学 | Molybdenum trioxide in-situ intercalation carbon nitride composite catalyst and preparation method thereof |
| CN115888788A (en) * | 2022-11-03 | 2023-04-04 | 常州大学 | Preparation method of three-dimensional honeycomb graphite phase carbon nitride composite photo-thermal catalyst, product and application thereof |
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