CN106732722A - A kind of preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure - Google Patents
A kind of preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure Download PDFInfo
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- CN106732722A CN106732722A CN201611132850.2A CN201611132850A CN106732722A CN 106732722 A CN106732722 A CN 106732722A CN 201611132850 A CN201611132850 A CN 201611132850A CN 106732722 A CN106732722 A CN 106732722A
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- 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
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention discloses a kind of preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure, carbon nitride photocatalyst has the 3-D ordered multiporous pattern of arranged regular, and macropore cavity is spherical, a diameter of 100nm~300nm;Two adjacent distances of the macropore centre of sphere are 110nm~350nm.The scanning electron microscope diagram piece of carbon nitride photocatalyst of the invention shows that it has the macroporous structure of three-dimensional order, and macropore cavity is spherical, a diameter of 100nm~300nm;Macroporous structure has specific surface area higher, and on the one hand the cavity of orderly macropore is interior can to load other materials, be on the other hand easy to mass transfer, can be with quick separating photo-generated carrier in reaction.The structure of carbon nitride photocatalyst of the invention has been obviously improved the photocatalysis performance of catalyst, under visible light with photocatalytic water H2-producing capacity higher, realizes efficient solar photolysis water hydrogen gas.
Description
The application is Application No. 201510085367.2, and the applying date is on 2 16th, 2015, and invention and created name is
The divisional application of the application for a patent for invention of " there is carbon nitride photocatalyst of three-dimensional ordered macroporous structure and preparation method thereof ".
Technical field
The invention belongs to photocatalysis technology field, and in particular to a kind of carbonitride light with three-dimensional ordered macroporous structure is urged
Agent and preparation method thereof.
Background technology
Conductor photocatalysis are that semiconductor catalyst produces electron-hole pair under visible ray or action of ultraviolet light, absorption
In the O of semiconductor surface2、H2O and contaminant molecule receive light induced electron or hole, and a series of redox reaction occurs
A kind of photochemical method.
Carbonitride is a kind of organic polymer semiconductor, because it has can be more stable in water with responding to visible light characteristic
And it is nontoxic, and the features such as preparation are easier, cause the extensive concern of researcher.Carbonitride is in photocatalysis, multiphase
The fields such as catalysis, fuel cell have potential application prospect, and water is especially catalytically decomposed under visible light conditions prepares hydrogen
On, carbonitride has the advantage of the uniqueness such as efficient, nontoxic, stable.
The pore structure on carbon nitride material surface and the size of specific surface area play highly important work on its application performance
With.At present, the common method for preparing carbonitride has fusion method, soft mode version method, die version method etc., and is obtained by various technologies
The nano materials such as nanometer sheet, nanometer rods, nanosphere, the mesoporous carbonitride of carbonitride are arrived.
Such as A of Chinese patent literature CN 103623856(Application number 201310663870.2)A kind of multistage is disclosed to receive
The spherical mesoporous carbon nitride photocatalyst of rice structure, described spherical mesoporous carbonitride has with nanometer sheet or similar nanometer sheet
Little particle is equably diffuseed to form the micro-nano structure that surface texture is highly opened wide, nanostructure height is stable from the centre of sphere to surrounding.
Preparation method is comprised the following steps:(1)The unlimited spherical mesoporous silica of synthetic surface structure height;(2)By spherical mesoporous
After high-temperature calcination removes organic matter, grinding adds watery hydrochloric acid to carry out acid treatment to silica under heating stirring, is centrifuged, and dries
It is dry, grinding;(3)In the flask containing suction filtration head, silica and cyanamide are added, under vacuum, ultrasonic and heating;Add water
Excessive cyanamide is centrifuged off, is dried;Solid powder is calcined into 2~8h in 723K~923K nitrogen furnaces high temperature;Use NH4HF2Solution
Etching removes silica template, and washing, drying obtains final product spherical mesoporous carbonitride.The spherical mesoporous for obtaining according to the method described above
Nitridation carbon surface has meso-hole structure, and specific surface area is larger, but synthetic method is complicated, synthesizes relatively costly, and mesoporous hole
Footpath is smaller, it is impossible to load the larger material of other particle diameters.
And such as A of Chinese patent literature CN 103721745(Application number 201410006468.1)Disclose a kind of copolymerization
The order mesoporous carbon nitride photocatalyst that is modified is closed, the described combined polymerization order mesoporous carbonitride that is modified has the microcosmic of cylindrical bar shape
The regular mesopore orbit of pattern and two-dimentional six sides P6mm ordered arrangements, light absorbs band edge is in 450nm~700nm.Preparation method bag
Include following steps:(1)Synthesize two-dimentional six sides P6mm SBA-15 type ordered mesoporous silica dioxides;(2)SBA-15 types order mesoporous two
After silica is through high-temperature calcination, grinding, watery hydrochloric acid being added while stirring in a heated condition, being centrifuged, sediment obtains sour through drying
Ordered mesoporous silica dioxide after change;(3)Ordered mesoporous silica dioxide after cyanamide, 3- aminothiophene -2- formonitrile HCNs and acidifying is mixed
Close, in a heated condition ultrasound and vacuumize;Add water centrifugation, dries, in 450 DEG C~650 DEG C nitrogen furnace high temperature thermopolymerizations 2~8
Hour;Silica template is removed with ammonium hydrogen fluoride solution, washing is dried, and obtains final product the modified order mesoporous carbonitride of combined polymerization.
Likewise, the order mesoporous carbonitride synthetic method that the combined polymerization disclosed in the patent document is modified is complicated, and it is relatively costly, it is mesoporous
Duct size is difficult to adjust, it is impossible to load the larger material of other particle diameters.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of carbonitride photocatalysis with three-dimensional ordered macroporous structure
Agent and preparation method thereof.
The technical scheme for realizing an object of the present disclosure is a kind of carbonitride photocatalysis with three-dimensional ordered macroporous structure
Agent, the 3-D ordered multiporous pattern with arranged regular, macropore cavity is spherical, a diameter of 100nm~300nm;Adjacent two
The distance of the individual macropore centre of sphere is 110nm~350nm.
The technical scheme for realizing the second purpose of the invention is a kind of carbonitride photocatalysis with three-dimensional ordered macroporous structure
The preparation method of agent, comprises the following steps:
1. the silica spheres array mould plate of three-dimensional order is prepared;Ethanol, water, ammoniacal liquor mixing and stirring are obtained into mixing molten
Liquid;To adding tetraethyl orthosilicate in mixed solution, after stirring 3~4 hours, the material centrifugation that will be obtained after reaction, remove from
Heart mother liquor, the precipitation that centrifugation is obtained is washed with ethanol, and drying obtains silica spheres;Ethanol, water, ammoniacal liquor, tetraethyl orthosilicate
Mass ratio be 50:(5~18)∶(2~6)∶(3~8).
By silica spheres ultrasonic disperse obtained above in ethanol, cover on the suspension surface for being obtained after ultrasonic disperse
Lid film, stands, and treats that suspension is evaporated into dry, and the white solid for obtaining is the silica ball array mould of three-dimensional order arrangement
Plate.
2. the preparation of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure;To in the white solid that 1. step obtains
Add cyanamide to obtain solidliquid mixture, then by solidliquid mixture feeding vacuum drying chamber, will be vacuumized in vacuum drying chamber,
The temperature inside the box is warming up to 55 DEG C~70 DEG C, is taken out after standing 2~4 hours, white solid is obtained after cooling, be intermediate A;Its
The white solid that 1. middle step obtains is 1: 1~3 with the mass ratio of cyanamide.
The intermediate A that will be obtained is put into tube furnace, and under nitrogen protection, holding 2~4 is small at 520 DEG C~550 DEG C
When, yellow powder is obtained after cooling, it is intermediate B.
Intermediate B is transferred in HF solution, stirring is centrifuged after 4~8 hours, and the precipitation being centrifugally separating to obtain is washed with water
Wash, the carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained final product after drying.
Used as preferred, 1. middle ethanol, water, ammoniacal liquor, the mass ratio of tetraethyl orthosilicate are 50 to above-mentioned steps:(5~
15)∶(2~5)∶(3~6).
As it is further preferred that above-mentioned steps 1. middle ethanol, water, ammoniacal liquor, tetraethyl orthosilicate mass ratio be 50:
(5~10)∶(2~4)∶(3~6).
The concentration of silica spheres is 25~50g/L in the suspension that 1. above-mentioned steps are obtained after middle ultrasonic disperse
Second technical scheme for realizing the second purpose of the invention is that a kind of carbonitride light with three-dimensional ordered macroporous structure is urged
The preparation method of agent, comprises the following steps:
1. the silica spheres array mould plate of three-dimensional order is prepared;Ethanol, water, ammoniacal liquor mixing and stirring are obtained into mixing molten
Liquid;To adding tetraethyl orthosilicate in mixed solution, after stirring 3~4 hours, the material centrifugation that will be obtained after reaction, remove from
Heart mother liquor, the precipitation that centrifugation is obtained is washed with ethanol, and drying obtains silica spheres;Ethanol, water, ammoniacal liquor, tetraethyl orthosilicate
Mass ratio be 50:(5~18)∶(2~6)∶(3~8).
By silica spheres ultrasonic disperse obtained above in ethanol, the suspension that will be obtained after ultrasonic disperse with
The speed high speed centrifugation of 8000r/min~10000r/min, the silica spherical array for obtaining three-dimensional order is dried after discarding ethanol
Row template.
2. the preparation of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure;To in the white solid that 1. step obtains
Add cyanamide to obtain solidliquid mixture, then by solidliquid mixture feeding vacuum drying chamber, will be vacuumized in vacuum drying chamber,
The temperature inside the box is warming up to 55 DEG C~70 DEG C, is taken out after standing 2~4 hours, white solid is obtained after cooling, be intermediate A;Its
The white solid that 1. middle step obtains is 1: 1~3 with the mass ratio of cyanamide.
The intermediate A that will be obtained is put into tube furnace, under nitrogen protection, is kept for 2~4 hours at 520~550 DEG C,
Yellow powder is obtained after cooling, is intermediate B.
Intermediate B is transferred in HF solution, stirring is centrifuged after 4~8 hours, and the precipitation being centrifugally separating to obtain is washed with water
Wash, the carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained final product after drying.
Used as preferred, 1. middle ethanol, water, ammoniacal liquor, the mass ratio of tetraethyl orthosilicate are 50 to above-mentioned steps:(5~
15)∶(2~5)∶(3~6).
As it is further preferred that above-mentioned steps 1. middle ethanol, water, ammoniacal liquor, tetraethyl orthosilicate mass ratio be 50:
(5~10)∶(2~4)∶(3~6).
The concentration of silica spheres is 80~120g/L in the suspension that 1. above-mentioned steps are obtained after middle ultrasonic disperse.
The present invention has positive effect:(1)The scanning electron microscope diagram piece of carbon nitride photocatalyst of the invention shows
Show that its microscopic appearance has the macroporous structure of three-dimensional order, macropore cavity is spherical, a diameter of 100nm~300nm;Macroporous structure
With specific surface area higher, on the one hand the cavity of orderly macropore is interior can to load other materials, be on the other hand easy to mass transfer,
Can be with quick separating photo-generated carrier in reaction.The structure of carbon nitride photocatalyst of the invention has been obviously improved the light of catalyst
Catalytic performance, under visible light with photocatalytic water H2-producing capacity higher, realizes efficient solar photolysis water hydrogen gas.
(2)The preparation method of carbon nitride photocatalyst of the invention prepares the silica of three-dimensional order arrangement first
Ball, it is poly- in protective gas high temperature with cyanamide as predecessor then using the three-dimensional ordered array of silica spheres as masterplate
Close, the carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained after finally removing silica with hydrofluoric acid.
(3)The size of the macropore diameter of carbon nitride photocatalyst of the invention is in preparation process by controlling silica
The size of ball can very easily be adjusted so that carbon nitride photocatalyst is adapted to the different size of other materials of load.When
When needing the volume of the other materials of load larger, the titanium dioxide of greater particle size is prepared when preparing carbon nitride photocatalyst first
Silicon ball, after finally removing silica spheres with hydrofluoric acid, obtained catalyst is the macropore with larger aperture, meets to apply and wants
Ask.
(4)Catalyst of the invention prepares that synthesis technique is simple, and stability is high, and the raw material for using is inexpensive.Obtained nitrogen
Change carbon photochemical catalyst and be free of metal, it is nontoxic, can recycle, with good practical value, have very well in photocatalysis field
Application prospect.
Brief description of the drawings
Fig. 1 is 5000 times of scanning electron microscope diagram pieces of carbon nitride photocatalyst prepared by embodiment 1;
Fig. 2 is 20000 times of scanning electron microscope diagram pieces of carbon nitride photocatalyst prepared by embodiment 1;
Fig. 3 is the X-ray diffractogram of carbon nitride photocatalyst prepared by embodiment 1, ordinate intensity- intensity in figure, figure
Middle abscissa degree- degree.
Fig. 4 is the photocatalysis Decomposition aquatic products hydrogen of the carbon nitride photocatalyst with common carbon nitride catalyst of the preparation of embodiment 1
Performance comparision figure, ordinate is hydrogen-producing speed.
Specific embodiment
(Embodiment 1)
The carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment is that a kind of organic polymer semiconductor light is urged
Agent, chemical formula is C3N4, preparation method comprises the following steps:
1. the silica spheres array mould plate of three-dimensional order is prepared.
By 60g ethanol, 12g water, 4g ammoniacal liquor(28wt%)Mixing and stirring obtains mixed solution;Add in mixed solution
Enter 6mL tetraethyl orthosilicates(CAS NO. 78-10-4), after stirring 3 hours, the centrifugation of the material that will be obtained after reaction, remove from
Heart mother liquor, the precipitation that obtains of centrifugation wash with ethanol, is then dried at 80 DEG C and is obtained silica spheres.
By silica spheres ultrasonic disperse obtained above in 80mL ethanol, the suspension table obtained after ultrasonic disperse
Face cover film, stands, and treats that suspension is slowly evaporated into dry, and the white solid for obtaining is the silica spheres of three-dimensional order arrangement
Array mould plate;The concentration of silica spheres is 25~50g/L wherein in suspension.
2. the preparation of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure.
To adding 2g cyanamides to obtain solidliquid mixture in the white solid that 1. step obtains, then solidliquid mixture is sent into
In vacuum drying chamber, will be vacuumized in vacuum drying chamber, the temperature inside the box is warming up to 60 DEG C, taken out after standing 4 hours, after cooling
White solid is obtained, is intermediate A;Cyanamide is sufficiently submerged in the silica ball array masterplate of three-dimensional order arrangement in intermediate A.
The intermediate A that will be obtained is put into tube furnace, under nitrogen protection, 550 DEG C is warming up to the speed of 4 DEG C/min,
Kept for 4 hours, yellow powder is obtained after cooling, be intermediate B.
Intermediate B is transferred to the HF solution of 10mL(16wt%)In, it is centrifuged after stirring 8h, the precipitation being centrifugally separating to obtain
Wash with water 3 times, the powdered carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained after drying.
Carbon nitride photocatalyst outward appearance with three-dimensional ordered macroporous structure manufactured in the present embodiment is pale yellow powder.
Product composition is characterized in D8-XRD types(German BRUKER companies production)Completed on X-ray diffractometer, Cu targets KαSpoke
Penetrate(λ=0.154056nm), 1.0 °/min of sweep speed, 0~80 ° of wide-angle diffraction measurement range.
The observation of pattern and granularity is in S-3400NII types(Japanese Hitachi companies production)SEM(SEM)
Under carry out.
See Fig. 1 and Fig. 2, scanning electron microscope diagram piece shows, carbon nitride photocatalyst obtained in the present embodiment has big
The 3-D ordered multiporous pattern of area arranged regular, macropore cavity is spherical, a diameter of 250nm~280nm.Adjacent macropore ball
The distance of the heart is 260nm~300nm.
See Fig. 3, what the XRD diffraction patterns of carbon nitride photocatalyst manufactured in the present embodiment confirmed that the present embodiment prepares is
The carbonitride of graphite-phase.
In order to check the carbon nitride photocatalyst photocatalysis Decomposition with three-dimensional ordered macroporous structure manufactured in the present embodiment
The performance of aquatic products hydrogen, the experiment of photocatalytic degradation water is carried out to it:Obtained carbon nitride photocatalyst is added into 100mL water
In, the concentration of carbon nitride photocatalyst is 1*10-3g/mL;Under visible light illumination, photolysis water hydrogen;With online gas-chromatography skill
Art carries out quantitative analysis to hydrogen output.
Test as a comparison, to adding common body phase carbonitride to compare in 100mL water, body phase carbon nitride photocatalyst
Concentration is 1*10-3g/mL;Under visible light illumination, photolysis water hydrogen;Hydrogen output is quantified with online gas chromatographic technique
Analysis.
Result is as shown in Figure 4:The obtained carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment(Fig. 4
In be referred to as three-dimensional ordered macroporous carbonitride)Hydrogen-producing speed is 142 μm of ol/h, and common body phase carbonitride hydrogen-producing speed is 7.8 μ
Mol/h, the H2-producing capacity of the obtained carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment is far above common
Body phase carbonitride, is 18 times of its hydrogen-producing speed.
(Embodiment 2)
Remaining is identical with embodiment for the preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment,
Difference is:
When 1. step prepares the silica spheres array mould plate of three-dimensional order, by 50g ethanol, 10g water, 3g ammoniacal liquor(28 wt%%)
Mixing and stirring obtains mixed solution, to addition 5mL tetraethyl orthosilicates in the mixed solution for obtaining, after stirring 4 hours, and will
The material centrifugation obtained after reaction, removes centrifuge mother liquor, and the precipitation that obtains of centrifugation is washed with ethanol, then dries at 80 DEG C and obtains
Silica spheres.
In 8mL ethanol, the suspension for obtaining is with the speed of 10000r/min for the silica spheres ultrasonic disperse that will be obtained
High speed centrifugation, the silica spheres array mould plate for obtaining three-dimensional order is dried after discarding ethanol;Silica spheres in suspension
Concentration is 80~120g/L.
Add 2.5g cyanamides to obtain solidliquid mixture in the white solid that 1. 2. step is obtained to step, then mix solid-liquid
In compound feeding vacuum drying chamber, will be vacuumized in vacuum drying chamber, the temperature inside the box is warming up to 70 DEG C, taken after standing 4 hours
Go out.
The intermediate B for obtaining is transferred to the HF solution of 8mL(16wt%)In, it is centrifuged after stirring 7h, what is be centrifugally separating to obtain is heavy
Shallow lake is washed with water 3 times, and the carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained final product after drying.
Carbon nitride photocatalyst obtained in the present embodiment has the 3-D ordered multiporous pattern of large area arranged regular, macropore
Cavity is spherical, a diameter of 200nm~250nm.Two adjacent distances of the macropore centre of sphere are 210nm~260nm.
According to the method for embodiment 1, the obtained carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment
Hydrogen-producing speed is 157 μm of ol/h.
(Embodiment 3)
Remaining is identical with embodiment for the preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment,
Difference is:
When 1. step prepares the silica spheres array mould plate of three-dimensional order, by 50g ethanol, 15 g water, 5g ammoniacal liquor(28wt%%)
Mixing and stirring obtains mixed solution, to addition 5mL tetraethyl orthosilicates in the mixed solution for obtaining.
Carbon nitride photocatalyst obtained in the present embodiment has the 3-D ordered multiporous pattern of large area arranged regular, macropore
Cavity is spherical, a diameter of 120nm~150nm.Two adjacent distances of the macropore centre of sphere are 130nm~160nm.
According to the method for embodiment 1, the obtained carbon nitride photocatalyst with three-dimensional ordered macroporous structure of the present embodiment
Hydrogen-producing speed is 160 μm of ol/h.
The scanning electron microscope diagram piece of carbon nitride photocatalyst of the invention shows that it has the macropore knot of three-dimensional order
Structure, macropore cavity is spherical, a diameter of 100nm~300nm;Macroporous structure has specific surface area higher, orderly macropore
Other materials on the one hand can be loaded in cavity, is on the other hand easy to mass transfer, can be with quick separating photo-generated carrier in reaction.This
The structure of the carbon nitride photocatalyst of invention has been obviously improved the photocatalysis performance of catalyst, under visible light with light higher
Solution water H2-producing capacity, realizes efficient solar photolysis water hydrogen gas.
Claims (2)
1. a kind of preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure, it is characterised in that including following step
Suddenly:
1. the silica spheres array mould plate of three-dimensional order is prepared;Ethanol, water, ammoniacal liquor mixing and stirring are obtained into mixing molten
Liquid;To adding tetraethyl orthosilicate in mixed solution, after stirring 3~4 hours, the material centrifugation that will be obtained after reaction, remove from
Heart mother liquor, the precipitation that centrifugation is obtained is washed with ethanol, and drying obtains silica spheres;Ethanol, water, ammoniacal liquor, tetraethyl orthosilicate
Mass ratio be 50:(5~15)∶(2~5)∶(3~6);
By silica spheres ultrasonic disperse obtained above in ethanol, silica spheres in the suspension obtained after ultrasonic disperse
Concentration be 80~120g/L, the suspension that will be obtained after ultrasonic disperse with the speed of 8000r/min~10000r/min at a high speed
Centrifugation, the silica spheres array mould plate for obtaining three-dimensional order is dried after discarding ethanol;
2. the preparation of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure;Added in the white solid that 1. step obtains
Cyanamide obtains solidliquid mixture, then by solidliquid mixture feeding vacuum drying chamber, will be vacuumized in vacuum drying chamber, by case
Interior temperature is warming up to 55 DEG C~70 DEG C, is taken out after standing 2~4 hours, and white solid is obtained after cooling, is intermediate A;Wherein walk
The rapid white solid for 1. obtaining is 1: 1~3 with the mass ratio of cyanamide;
The intermediate A that will be obtained is put into tube furnace, under nitrogen protection, is kept for 2~4 hours at 520~550 DEG C, cooling
After obtain yellow powder, be intermediate B;
Intermediate B is transferred in HF solution, stirring is centrifuged after 4~8 hours, and the precipitation being centrifugally separating to obtain is washed with water, is dried
The carbon nitride photocatalyst with three-dimensional ordered macroporous structure is obtained final product after dry.
2. the preparation method of the carbon nitride photocatalyst with three-dimensional ordered macroporous structure according to claim 1, it is special
Levy and be:1. middle ethanol, water, ammoniacal liquor, the mass ratio of tetraethyl orthosilicate are 50 to step:(5~10)∶(2~4)∶(3~6).
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CN109261191A (en) * | 2018-11-06 | 2019-01-25 | 武汉科技大学 | A kind of graphite phase carbon nitride foam catalysis material and preparation method thereof |
CN109261191B (en) * | 2018-11-06 | 2021-07-20 | 武汉科技大学 | Graphite phase carbon nitride foam photocatalytic material and preparation method thereof |
CN110721710A (en) * | 2019-10-21 | 2020-01-24 | 大连理工大学 | Ordered macroporous non-metal catalyst and preparation method thereof |
CN110721710B (en) * | 2019-10-21 | 2021-06-08 | 大连理工大学 | Ordered macroporous non-metal catalyst and preparation method thereof |
CN114452989A (en) * | 2022-01-30 | 2022-05-10 | 江苏大学 | Porous structure carbon nitride composite catalyst and preparation method and application thereof |
CN115888784A (en) * | 2022-10-18 | 2023-04-04 | 廊坊师范学院 | Carbon nitride photocatalyst with wide spectral response and preparation method thereof |
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