CN108993563A - A kind of preparation method of the three-dimensional network frame of montmorillonite and graphite phase carbon nitride - Google Patents
A kind of preparation method of the three-dimensional network frame of montmorillonite and graphite phase carbon nitride Download PDFInfo
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- CN108993563A CN108993563A CN201810705483.3A CN201810705483A CN108993563A CN 108993563 A CN108993563 A CN 108993563A CN 201810705483 A CN201810705483 A CN 201810705483A CN 108993563 A CN108993563 A CN 108993563A
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 49
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 38
- 239000010439 graphite Substances 0.000 title claims abstract description 38
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 13
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001338 self-assembly Methods 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000010792 warming Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001727 in vivo Methods 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- -1 is 1 calculating Chemical compound 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 239000011148 porous material Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000009830 intercalation Methods 0.000 abstract description 3
- 230000002687 intercalation Effects 0.000 abstract description 3
- 238000006068 polycondensation reaction Methods 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000012298 atmosphere Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229960000789 guanidine hydrochloride Drugs 0.000 description 1
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003863 metallic catalyst Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000012552 review Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005829 trimerization reaction Methods 0.000 description 1
- 239000003643 water by type 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/651—50-500 nm
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses the preparation methods of a kind of montmorillonite and the three-dimensional network frame of graphite phase carbon nitride, belong to the preparation field of porous material.Montmorillonite, cyanuric acid and melamine are added in the reaction kettle taken water as a solvent for invention, stir under fixed temperature and are dried to obtain presoma.Presoma is placed in have and is passed through in the furnace body of gas function, gas flow rate is controlled and heating rate is calcined, obtain montmorillonite and graphite phase carbon nitride three-dimensional network frame material compound layer by layer.The invention has the advantages that: melamine cyanurate is self-assembly of in the solution with melamine and cyanuric acid, and it is intercalation between montmorillonite layer, then as the carbon source of graphite phase carbon nitride and nitrogen source, thermal polycondensation reaction is generated by calcining in inert gas, prepare montmorillonite and graphite phase carbon nitride composite material layer by layer, and the method for the mass ratio of changeable raw material controls three-dimensional network frame aperture, process is simple.
Description
Technical field
The present invention relates to the preparation methods of a kind of montmorillonite and the three-dimensional network frame of graphite phase carbon nitride, belong to porous material
The preparation field of material can be used for the fields such as photocatalysis field and lithium ion battery negative material.
Background technique
Montmorillonite is the 2:1 structure multilayer silicate clay formed by oxygen-octahedron and alumina octahedral, wherein alumina
Part Al atom in octahedron is replaced by Mg, makes lamella with elecrtonegativity, interlayer is usually by Na+、Ca2+Equal metal cations are flat
Weigh charge.Each montmorillonite layer has comprising three sub-layers, and upper layer and lower layer are oxygen-octahedron sub-layer, and centre is alumina octahedral
Body sub-layer is connected between sub-layer with covalent bond by sharing oxygen atom, and only has faint Van der Waals force between adjacent sheets.It covers
De- soil is used as a kind of clay mineral, has the characteristics that cheap and easy to get, cation exchange capacity is big, is easy to intercalation.Graphite-phase nitridation
Carbon (graphitic carbon nitride), is abbreviated as g-C3N4, it is nitridation carbon allotrope the most stable, is a kind of
Very promising non-metallic catalyst.The fields such as the hydrogen manufacturing of the photodegradation that has been widely used water, photocatalysis.Because it has excellent performance
And it receives significant attention.
The lower thermal polycondensation reaction using melamine cyanurate super-molecule assembling body in hot conditions can effectively make at present
Obtaining graphite phase carbon nitride, (23 (29): Adv.Funct.Mater.2013 3661-3667.), can induce stronger with its layer structure
Light absorption, band gap can effectively increase 0.16eV.Three-dimensional netted frame structure has high-specific surface area and duct abundant, energy
More active points are exposed, reactant and product in the performances and heterogeneous reaction of applications such as catalysis reaction are then lifted at
Mass transfer diffusion.Framework material of the montmorillonite as three-dimensional network frame, come into full contact with graphite phase carbon nitride can be formed it is heterogeneous
Knot, because of the difference of its conduction band and valence band, graphite phase carbon nitride can be transferred to compound due to the electronics of light excitation generation or hole
Conduction band or valence band in, electron hole separation, recombination rate reduce, so as to more efficiently utilize light excitation generate active grain
Son improves catalytic efficiency (Chemical Reviews, 2016,116 (12): 7159-7329.).
Currently without the patent for imvite modified preparation three-dimensional network frame structure.Now use melamine cyanurate
Salt has imvite modified patent: a kind of melamine cyanurate and montmorillonite nano complex and preparation method thereof are (public
The number of opening: CN 104829860A, on August 12nd, 2015, Beijing Institute of Technology), it is added using melamine, cyanuric acid and urea
Into the reaction kettle containing montmorillonite and solvent, reaction obtains the nano-complex of melamine cyanurate and montmorillonite, uses
In polymer material flame retardant area.
The patent of preparation graphite phase carbon nitride has: a kind of method (publication number: CN preparing graphite phase carbon nitride material
106540733A, on March 29th, 2017, Institutes Of Technology Of Taiyuan), it the use of dicyanodiamine and nano silica is presoma, with
The graphitic carbon nitride of high specific surface area is prepared in microwave calcining and Muffle furnace roasting.A kind of conjunction of porous graphite phase carbon nitride
At method (publication number: CN104843658A, on August 19th, 2015, Changzhou University), with polystyrene or poly-methyl methacrylate
Ester microemulsion is hard template, and cyanamide, dicyanodiamine or guanidine hydrochloride are presoma, dry by directly mixing, the gas of inert gas
Porous graphite phase carbon nitride can be obtained in roasting under atmosphere.
Summary of the invention
The object of the present invention is to provide the preparation methods of a kind of montmorillonite and the three-dimensional network frame of graphite phase carbon nitride.It should
Composite material can be used for the fields such as photocatalysis field and lithium ion battery negative material as porous material.Application prospect is wide
It is wealthy, and preparation method process is simple, can be mass-produced.
The present invention is realized by following technological means, a kind of montmorillonite and graphite phase carbon nitride composite wood layer by layer
The three-dimensional network frame of material, which is characterized in that the three-dimensional network frame is stratiform montmorillonite-based nano piece and graphite phase carbon nitride layer
A kind of three-dimensional network frame structure that layer is compound and is built into, network aperture are 5-300nm, are with the gross mass of compound
100% calculates, and the mass percentage of montmorillonite is 50%-95%, and the mass percentage of graphite phase carbon nitride is 5%-
50%.
The preparation method of the montmorillonite of above structure and graphite phase carbon nitride the three-dimensional network frame of composite material layer by layer,
Be characterized in that the following steps are included:
(1) montmorillonite, melamine and cyanuric acid are added in the reaction kettle taken water as a solvent, it is small that 4 is stirred under fixed temperature
When, it removes solvent and is dried to obtain presoma.Wherein montmorillonite be unmodified montmorillonite perhaps organic modification montmonrillonite or
It is the clay containing montmorillonite structure, which only includes montmorillonite and melamine cyanurate, with the quality of montmorillonite
It is calculated for 1, the mass ratio of melamine cyanurate is 0.05~20.Melamine cyanurate by etc. amount of substance trimerization
H-bonding self-assembly obtains cyanamide in aqueous solution with cyanuric acid.The fixed temperature range of reaction is room temperature~100 DEG C, Optimal Temperature
It is 90 DEG C.
(2) by presoma made from step (1) be placed in tube furnace, Muffle furnace or other have be passed through gas function can heating furnace
In vivo, protective gas is passed through with certain gas flow rate into furnace body and started to warm up.The gas flow and heating speed being kept fixed
Rate is warming up to fixed temperature, keeps the temperature and calcines 30~200 minutes, it is compound layer by layer with graphite phase carbon nitride to obtain montmorillonite
The three-dimensional network frame of material.Protective gas is nitrogen (N2), argon gas (Ar) or helium (He).Gas flow be 100~
400ml/min, wherein optimal gas flow is 200ml/min.Heating rate is 1~50 DEG C/min, and optimal heating rate value is situated between
In 10~30 DEG C/min.Fixed temperature is 300~700 DEG C.
The advantages and positive effects of the present invention are: making melamine and cyanuric acid due to taking above-mentioned technical proposal
H-bonding self-assembly forms melamine cyanurate between montmorillonite layer, between achieving the effect that intercalation enters cheating engaging layer.Lead to again
Crossing inert gas shielding and temperature control heating makes melamine cyanurate thermal polycondensation graphite phase carbon nitride.It is covered by control de-
The pore size of soil and melamine cyanurate mass ratio control three-dimensional network frame.This method is low in cost, reacts
Journey is simple, and controllability is strong.
Detailed description of the invention
Fig. 1 is the three-dimensional network frame of the composite material layer by layer of montmorillonite and graphite phase carbon nitride made from present example 3
Electron scanning micrograph.From this view it is apparent that the material three-dimensional network frame structure.
Specific embodiment
Below by example, the invention will be further described, but embodiment is not intended to limit protection scope of the present invention.It is (each
Raw material is that commercially available analysis is pure)
Embodiment 1
0.556 gram of montmorillonite is weighed, 0.735 gram of melamine, 0.692 gram of cyanuric acid, 1000ml milliliters has been added to and has gone
In the reaction kettle of ionized water, 95 DEG C of stirring 3h are warming up to, filter to obtain precursor product, 80 DEG C of vacuum drying 4h.Presoma is set
In tube furnace, it is passed through gas flow rate and is the argon gas of 500ml/min, and temperature is warming up to the heating rate of 2.3 DEG C/min
550 DEG C of degree keeps the temperature 1h.It is cooled to room temperature under argon atmosphere protection after reaction, obtains montmorillonite and graphite phase carbon nitride
The three-dimensional network frame of composite material layer by layer, measuring product aperture made from the formula is 50nm.
Embodiment 2
0.581 gram of cation-modified montmorillonite is weighed, 1.235 grams of melamine, 1.196 grams of cyanuric acid, has been added to
In the reaction kettle of 1000 ml deionized waters, 80 DEG C of stirring 4h are warming up to, rotary evaporation obtains precursor product.Presoma is set
In tube furnace, it is passed through the nitrogen gas that gas flow rate is 300ml/min, temperature is warming up to the heating rate of 10 DEG C/min
650 DEG C, keep the temperature 1h.It is cooled to room temperature under nitrogen atmosphere protection after reaction, obtains montmorillonite and graphite phase carbon nitride layer
The three-dimensional network frame of layer composite material, measuring product aperture made from the formula is 20nm.
Embodiment 3
Weigh 0.501 gram of montmorillonite, 0.595 gram of melamine, 0.612 gram of cyanuric acid, be added to 1000 milliliters go from
In the reaction kettle of sub- water, 70 DEG C of stirring 4h are warming up to, filter to obtain precursor product, 80 DEG C of vacuum drying 4h.Presoma is placed in
In tube furnace, it is passed through the helium atmosphere that gas flow rate is 100ml/min, temperature 650 is warming up to the heating rate of 50 DEG C/min
DEG C, keep the temperature 1h.It is cooled to room temperature under helium atmosphere protection after reaction, it is multiple layer by layer to obtain montmorillonite and graphite phase carbon nitride
The three-dimensional network frame of condensation material, measuring product aperture made from the formula is 100nm.
Claims (12)
1. a kind of preparation method of the three-dimensional network frame of montmorillonite and graphite phase carbon nitride, the preparation method include following step
It is rapid: (1) montmorillonite, melamine and cyanuric acid to be added in the reaction kettle taken water as a solvent, it is small that 4 are stirred under fixed temperature
When, it removes solvent and is dried to obtain presoma.
2. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 1 and graphite phase carbon nitride,
Be characterized in that: the montmorillonite that raw material uses is unmodified montmorillonite or organic modification montmonrillonite, or contains montmorillonite
The clay of structure.
3. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 1 and graphite phase carbon nitride,
Be characterized in that: the presoma includes montmorillonite and melamine cyanurate, is 1 calculating, melamine with the quality of montmorillonite
The mass ratio of cyanurate be 0.05~20, wherein melamine cyanurate by etc. amount of substance melamine and cyanuric acid
H-bonding self-assembly obtains in aqueous solution.
4. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 1 and graphite phase carbon nitride,
Be characterized in that: the range of fixed temperature is room temperature~100 DEG C in reaction process, and Optimal Temperature is 90 DEG C.
5. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 1 and graphite phase carbon nitride,
Be characterized in that: removal dissolving agent process includes natural drying, suction filtration or rotary evaporation in vacuo.
6. a kind of preparation method of the three-dimensional network frame of montmorillonite and graphite phase carbon nitride, the preparation method include following step
It is rapid: (2) by presoma made from step (1) be placed in tube furnace, Muffle furnace or other have be passed through gas function can heating furnace
In vivo, protective gas is passed through with certain gas flow rate into furnace body and started to warm up, the gas flow being kept fixed and heating speed
Rate is warming up to fixed temperature, keeps the temperature and calcines a period of time, obtains montmorillonite and graphite phase carbon nitride composite wood layer by layer
The three-dimensional network frame of material.
7. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: place step (1) presoma furnace body be tube furnace, Muffle furnace or other with controllable heating rate and can lead to
Enter the furnace body of gas function.
8. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: the protective gas being passed through into furnace body is nitrogen (N2), argon gas (Ar) or helium (He).
9. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: the gas flow that protective gas is passed through into furnace body is 100~400ml/min, wherein optimal gas flow is
200ml/min。
10. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: heating rate is 1~50 DEG C/min in temperature-rise period, and optimal heating rate value is between 10~30 DEG C/min.
11. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: furnace body is warming up to fixed temperature, which is 300~700 DEG C.
12. the preparation method of the three-dimensional network frame of a kind of montmorillonite according to claim 6 and graphite phase carbon nitride,
Be characterized in that: the calcination time under fixed temperature is 30~200min.
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CN110026221A (en) * | 2019-04-26 | 2019-07-19 | 沈阳建筑大学 | A kind of montmorillonite-base optic catalytic composite material and preparation method thereof |
CN110075901A (en) * | 2019-05-14 | 2019-08-02 | 东南大学 | Porous sulphur mixes the preparation of graphite phase carbon nitride-redox graphene nanometer sheet |
CN110142057A (en) * | 2019-05-17 | 2019-08-20 | 浙江工业大学 | A kind of Ag/g-C3N4/ bamboo charcoal/montmorillonite composite material and its application |
CN110560120A (en) * | 2019-08-16 | 2019-12-13 | 徐州工程学院 | Preparation method of porous carbon nitride material, porous carbon nitride material and application thereof |
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