CN108355698A - A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder - Google Patents

A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder Download PDF

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Publication number
CN108355698A
CN108355698A CN201810148643.9A CN201810148643A CN108355698A CN 108355698 A CN108355698 A CN 108355698A CN 201810148643 A CN201810148643 A CN 201810148643A CN 108355698 A CN108355698 A CN 108355698A
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nanometer sheet
preparation
sheet powder
carbon nitride
phase carbon
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孙少东
梁淑华
李佳
苟旭峰
崔杰
杨卿
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Xian University of Technology
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Xian University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • B01J35/39

Abstract

The invention discloses a kind of preparation methods of O doped graphites phase carbon nitride nanometer sheet powder, make raw material with melamine, hydrogen peroxide and water, and modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then the melamine of above-mentioned modification is subjected to high-temperature calcination, you can obtain broad stopband O doping g C3N4Nanometer sheet powder.Obtained O doping g C3N4Nanometer sheet powder compares body phase g C3N4With higher specific surface area, while O is incorporated into g C3N4Conventional bulk phase g C are changed in skeleton3N4Electronic structure so that energy gap significantly increases, while overcoming it to light induced electron and hole easily quick compound, disadvantage that photo-quantum efficiency is low, to improve g C3N4Photocatalysis performance.And the method for 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

A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder
Technical field
The invention belongs to catalysis material preparing technical fields, and in particular to a kind of O doped graphites phase carbon nitride nanometer sheet The preparation method of powder.
Background technology
Graphite phase carbon nitride (g-C3N4) make a kind of novel polymer semiconductor's photochemical catalyst and closed extensively by people Note.Numerous studies show at present:g-C3N4With lamellar structure, suitable band structure and goodization similar to graphene Stability is learned, therefore in photocatalytic pollutant degradation, decomposition aquatic products hydrogen and reduction CO2Field has a good application prospect.So And conventional bulk phase g-C3N4Specific surface area is small and photo-generated carrier is easy and fast to compound disadvantage and significantly limits its light to urge Change performance.
g-C3N4Physical and chemical performance and its microstructure and electronic structure it is closely related.Conventional g-C3N4Catalysis material Modification mode includes mainly:Morphological control, carried noble metal and metal/non-metal doping.In particular, doping vario-property passes through two Tie up stratiform g-C3N4Layer in and interlayer introduce heteroatom so that foreign atom track and g-C3N4Original molecular orbit hair Raw Orbit revolutionary, can cause the change of electronic structure, lead to g-C3N4Material is realized in the variation of valence band and conduction level position Visible light utilization efficiency and photocatalytic redox potential optimization, and then improve its photocatalysis performance.In recent years, O adulterates g- C3N4It gets more and more people's extensive concerning, the increase of photocatalytic redox potential may be implemented in element doping strategy, to effectively carry The photocatalysis performance of high material.However, related broad stopband O adulterates g-C at present3N4The still rare document report of research.
Therefore, the present invention provides a kind of modifies preparation O of forerunner to adulterate g-C3N4Strategy selects melamine, double first Oxygen water and water make raw material, and modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then The melamine of above-mentioned modification is subjected to high-temperature calcination, you can obtain broad stopband O and adulterate g-C3N4Nanometer sheet powder.
Invention content
The object of the present invention is to provide a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, solve existing There is g-C3N4To the easily quick problem compound, photo-quantum efficiency is low in light induced electron and hole, and improve its energy gap.
The technical solution adopted in the present invention is a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, tool Body is implemented according to the following steps:
Step 1, the preparation of modified presoma:
Melamine, hydrogen peroxide, 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, O adulterates g-C3N4The preparation of nanometer sheet powder:
The modification presoma obtained to step 1 carries out high-temperature calcination to get to g-C3N4Nanometer sheet powder.
Feature of the present invention also resides in,
Melamine and the mass volume ratio of deionized water are 1 in step 1:60~1:1, the body of hydrogen peroxide and deionized water Product is than being 1:60~1:1.
The mass concentration of hydrogen peroxide is 30% in step 1.
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 0.5~6h.
Heating rate is 0.1~10 DEG C/min in calcination process.
The invention has the advantages that the present invention makees raw material, hydrothermal treatment and height with melamine, hydrogen peroxide and water Temperature calcining obtains broad stopband O doping g-C3N4Nanometer sheet powder.Used hydrogen peroxide auxiliary hydro-thermal process presoma strategy at Realize g-C to work(3N4The band structure of powder is modified, and the O of acquisition adulterates g-C3N4Nanometer sheet powder compares body phase g-C3N4Tool There is higher specific surface area, while O is incorporated into g-C3N4Conventional bulk phase g-C is changed in skeleton3N4Electronic structure so that prohibit Bandwidth significantly increases, while overcoming it to light induced electron and hole easily quick compound, disadvantage that photo-quantum efficiency is low, from And improve g-C3N4Photocatalysis performance.And the method for the present invention is simple, easily controllable with reaction process, uses cost of material It is low, to equipment without particular/special requirement the advantages of, fully catered to the industrial scale applications of simple and environmentally-friendly low cost instantly, be suitble to extensive Industrialized production.
Description of the drawings
Fig. 1 is O doping g-C prepared by the embodiment of the present invention 13N4The transmission electron micrograph of nanometer sheet powder;
Fig. 2 is O 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 O doped graphites phase carbon nitride nanometer sheet powder of the present invention, with melamine, hydrogen peroxide and water Make raw material, modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then change above-mentioned Property melamine carry out high-temperature calcination, you can obtain broad stopband O adulterate g-C3N4Nanometer sheet powder.
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, addition mass concentration is 30% hydrogen peroxide, After mixing, deionized water is added, the mass ratio of melamine and deionized water is 1:60~1:1, hydrogen peroxide and deionized water Volume ratio is 1:60~1:1, it is to be mixed uniform, it closes the lid and moves it into corresponding stainless steel cauldron housing, in an oven 120~200 DEG C of 12~96h of heat preservation, the presoma solidliquid mixture deionized water and absolute ethyl alcohol that are obtained are centrifuged respectively Cleaning 3~6 times, what is obtained is deposited in 50~90 DEG C of dry 12~36h, you can obtains the melamine forerunner that hydrogen peroxide is modified Body.
Step 2, O adulterates g-C3N4The preparation of nanometer sheet powder:
The melamine presoma that the hydrogen peroxide that step 1 is obtained is modified, is put into alumina crucible, closes the lid;With 500 DEG C in air atmosphere~600 DEG C 0.5~6h of calcining of Muffle furnace, calcining heating rate is 0.1~10 DEG C/min.It can obtain It obtains O and adulterates 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, using hydrogen peroxide auxiliary hydro-thermal process presoma successfully realize g-C3N4The band structure of powder is modified, and is led to The volume ratio of hydrogen peroxide and deionized water in adjustment and control system is crossed, the O with different doping O contents can be prepared and adulterate g-C3N4 Nanometer sheet powder improves conventional bulk phase g-C3N4Powder is easy to reunite and the unconspicuous structural disadvantages of two-dimensional structure.It is obtained The O doping g-C obtained3N4Nanometer sheet powder compares body phase g-C3N4With higher specific surface area, while O is incorporated into g-C3N4 Conventional bulk phase g-C is changed in skeleton3N4Electronic structure so that energy gap significantly increases, at the same overcome its to photoproduction electricity Son and the easily quick disadvantage compound, photo-quantum efficiency is low in hole, to improve g-C3N4Photocatalysis performance.System of the present invention The O obtained adulterates g-C3N4Hydrogen-producing speed (1050.3 μm of olg of nanometer sheet-1·h-1) more unmodified melamine dinectly bruning institute The body phase g-C of acquisition3N4Hydrogen-producing speed (98.2 μm of olg-1·h-1) improve nearly 10.7 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 deionized mass ratio:10, mass concentration be 30% hydrogen peroxide and go from The volume ratio of sub- water is 1:60, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 140 DEG C 12h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 3 times with deionized water and absolute ethyl alcohol, finally exists Dry 36h in 50 DEG C of baking ovens, you can obtain modified cyanurotriamide 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 0.5 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
The O 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 deionized mass ratio:1, mass concentration be 30% hydrogen peroxide and go from The volume ratio of sub- water is 1:1, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, stirred It mixes uniformly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 180 DEG C 36h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 6 times with deionized water and absolute ethyl alcohol, finally exists Dry 12h in 90 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 550 DEG C of isothermal holdings 3h, calcining heating rate are 3 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
The O 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 deionized mass ratio:5, mass concentration be 30% hydrogen peroxide and go from The volume ratio of sub- water is 1:10, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 200 DEG C For 24 hours, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 4 times with deionized water and absolute ethyl alcohol, finally exists Dry 18h in 70 DEG C of baking ovens, you can obtain modified cyanurotriamide 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 10 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
Embodiment 4
Step 1, it is 1 according to melamine and deionized mass ratio:30, mass concentration be 30% hydrogen peroxide and go from The volume ratio of sub- water is 1:5, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, stirred It mixes uniformly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 120 DEG C 96h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 3 times with deionized water and absolute ethyl alcohol, finally exists Dry 15h in 60 DEG C of baking ovens, you can obtain modified cyanurotriamide 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 5 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
Embodiment 5
Step 1, it is 1 according to melamine and deionized mass ratio:60, mass concentration be 30% hydrogen peroxide and go from The volume ratio of sub- water is 1:10, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 160 DEG C 72h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 5 times with deionized water and absolute ethyl alcohol, finally exists Dry 30h in 60 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 580 DEG C of isothermal holdings 0.5h, calcining heating rate are 0.1 DEG C/min, you can obtain O and adulterate g-C3N4Powder.

Claims (8)

1. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, which is characterized in that specifically real according to the following steps It applies:
Step 1, the preparation of modified presoma:
Melamine, hydrogen peroxide, deionized water are added in reaction kettle, is stirred evenly, is put into baking oven and carries out hydro-thermal reaction, obtain To solidliquid mixture;Then solidliquid mixture washed, dried, obtain modified presoma;
Step 2, O adulterates g-C3N4The preparation of nanometer sheet powder:
The modification presoma obtained to step 1 carries out high-temperature calcination to get to g-C3N4Nanometer sheet powder.
2. a kind of preparation method of O 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 1:60~1:1, the volume ratio of hydrogen peroxide and deionized water It is 1:60~1:1.
3. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist In the mass concentration of hydrogen peroxide is 30% in the step 1.
4. a kind of preparation method of O 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.
5. a kind of preparation method of O 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.
6. a kind of preparation method of O 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.
7. a kind of preparation method of O 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 0.5~6h.
8. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1 or claim 7, feature It is, heating rate is 0.1~10 DEG C/min in the calcination process.
CN201810148643.9A 2018-02-13 2018-02-13 A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder Pending CN108355698A (en)

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CN111232939A (en) * 2020-01-17 2020-06-05 南京工业大学 Easier-to-peel g-C prepared by embedding stereo molecules3N4Method (2)
CN112547109A (en) * 2020-12-24 2021-03-26 江苏大学 Preparation method of wide-spectrum response type three-dimensional carbon nitride photocatalyst for carbon and oxygen co-doping by introducing polymer molecules
CN113000061A (en) * 2021-03-04 2021-06-22 西北工业大学 Preparation method of strip-shaped graphite carbon nitride nanosheet
CN114797937A (en) * 2022-04-22 2022-07-29 湖南大学 Filled mesoporous-rich tubular carbon nitride photocatalyst and preparation method and application thereof

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CN109569691A (en) * 2018-12-23 2019-04-05 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of boron doping carbonitride and products thereof and application
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CN109607500A (en) * 2018-12-29 2019-04-12 广西大学 A kind of g-C3N4The preparation method of ultrathin nanometer piece
CN110201698A (en) * 2019-06-03 2019-09-06 肇庆市华师大光电产业研究院 A kind of preparation method of polynary nonmetal doping carbon nitride photocatalyst
CN110342477A (en) * 2019-06-10 2019-10-18 西安理工大学 A kind of oxygen doping nitride porous carbon nanosheet and preparation method thereof
CN111036275B (en) * 2020-01-07 2022-08-05 南开大学 Preparation and application method of oxygen-doped graphite-phase nitrogen carbide photolysis water-hydrogen production catalyst
CN111036275A (en) * 2020-01-07 2020-04-21 南开大学 Preparation and application method of oxygen-doped graphite-phase nitrogen carbide photolysis water-hydrogen production catalyst
CN111232939A (en) * 2020-01-17 2020-06-05 南京工业大学 Easier-to-peel g-C prepared by embedding stereo molecules3N4Method (2)
CN111232939B (en) * 2020-01-17 2023-06-09 南京工业大学 Preparation of g-C with easier stripping by stereo molecule embedding 3 N 4 Is a method of (2)
CN112547109A (en) * 2020-12-24 2021-03-26 江苏大学 Preparation method of wide-spectrum response type three-dimensional carbon nitride photocatalyst for carbon and oxygen co-doping by introducing polymer molecules
CN112547109B (en) * 2020-12-24 2023-07-18 江苏大学 Preparation method of carbon-oxygen co-doped broad-spectrum response three-dimensional carbon nitride photocatalyst by introducing polymer molecules
CN113000061B (en) * 2021-03-04 2023-05-23 西北工业大学 Preparation method of banded graphite carbon nitride nanosheets
CN113000061A (en) * 2021-03-04 2021-06-22 西北工业大学 Preparation method of strip-shaped graphite carbon nitride nanosheet
CN114797937A (en) * 2022-04-22 2022-07-29 湖南大学 Filled mesoporous-rich tubular carbon nitride photocatalyst and preparation method and application thereof

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Application publication date: 20180803