CN107185576A - A kind of preparation method of carbonitride/graphene composite material of three-dimensional structure - Google Patents
A kind of preparation method of carbonitride/graphene composite material of three-dimensional structure Download PDFInfo
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- CN107185576A CN107185576A CN201710370895.1A CN201710370895A CN107185576A CN 107185576 A CN107185576 A CN 107185576A CN 201710370895 A CN201710370895 A CN 201710370895A CN 107185576 A CN107185576 A CN 107185576A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000002023 wood Substances 0.000 claims description 4
- 238000002242 deionisation method Methods 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 5
- OQVYMXCRDHDTTH-UHFFFAOYSA-N 4-(diethoxyphosphorylmethyl)-2-[4-(diethoxyphosphorylmethyl)pyridin-2-yl]pyridine Chemical compound CCOP(=O)(OCC)CC1=CC=NC(C=2N=CC=C(CP(=O)(OCC)OCC)C=2)=C1 OQVYMXCRDHDTTH-UHFFFAOYSA-N 0.000 abstract 1
- 238000010790 dilution Methods 0.000 abstract 1
- 239000012895 dilution Substances 0.000 abstract 1
- 238000004108 freeze drying Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 5
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- 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
-
- B01J35/23—
-
- B01J35/39—
-
- 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
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
-
- 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
- B01J37/12—Oxidising
-
- 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
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of preparation method of carbonitride/graphene composite material of three-dimensional structure, its step：（1) graphene oxide solution is prepared with Hummers methods；（2) dicyandiamide is put into Muffle furnace, carbonitride (g C is made3N4）；By carbonitride (g C3N4）Add to concentrated sulfuric acid solution stirring, sodium nitrate and potassium manganate stirring are then added under ice bath；Diluted, dialysed after dilution with deionized water and hydrogen peroxide, then be placed at~55 DEG C dry obtained carbonitride（g‑C3N4）；（3) carbonitride that graphene oxide (GO) solution for obtaining step (1) is obtained with step (2)（g‑C3N4）Nanometer sheet is 5 in mass ratio：3 ultrasonic mixings are uniform, ethylenediamine added, in 95 DEG C of isothermal reactions；CTAB solution is added to after above-mentioned reaction 7h is reacted in solution, take out product, washing, freeze-drying obtain carbonitride/graphene composite material of three-dimensional structure.The composite of the three-dimensional structure, adds ethylenediamine with CTAB as bridging agent, can improve the retractility and stability of the composite.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, carbonitride/graphene of more particularly to a kind of three-dimensional structure
The preparation method of composite.
Background technology
Since finding graphene from 2004, the extensive concern of researcher has just been caused.Graphene is in microelectronics, energy
Amount storage, is catalyzed, and there is great potential using value in the field such as biology sensor.Because it has two-dimensional nanostructure so that
With the addition of the composite of graphene often has high thermal conductivity, high specific surface area performance and high electric conductivity.
Carbonitride (g-C3N4) had a good application prospect as a kind of nonmetallic visible-light photocatalyst, due to nitridation
Carbon (g-C3N4) itself there is the layer structure of similar graphite, can be by chemical method by carbonitride (g-C3N4) peel off into individual layer
The structure of sheet, makes it have the excellent properties of similar graphene, possesses efficiently excellent photocatalysis property.But, the nitridation
Carbon (g-C3N4) still have several drawbacks part：Specific surface area is smaller；Band gap width is relatively large；Light induced electron and hole separation
Degree is not high.
The content of the invention
It is an object of the invention to provide a kind of preparation method of carbonitride/graphene composite material of three-dimensional structure, plus
Enter ethylenediamine with CTAB as bridging agent, the retractility and stability of the composite can be improved.
To reach above-mentioned purpose, the present invention is adopted the following technical scheme that：
The preparation method of carbonitride/graphene composite material of a kind of three-dimensional structure, it is characterised in that comprise the steps of：
(1) prepares graphene oxide (GO) using Hummers methods：The graphene oxide solution of certain volume is taken, water is used
1~5mg/ml of concentration is diluted to, 0.5~2h is stirred, obtains graphene oxide (GO) solution；
(2) preparation of carbonitrides (g-C3N4) nanometer sheet：
5~20g dicyandiamide is put into Muffle furnace by (2-1) is warming up to 550 DEG C, is incubated 2~4 h, carbonitride (g- is made
C3N4)；
(2-2) is by above-mentioned gained carbonitride (g-C3N4) add into 100mL concentrated sulfuric acid solution, stirred under agitator
20~24h, then, under condition of ice bath, sequentially adds 1g sodium nitrate (NaNO3) and 10g potassium permanganate (KMnO4), 8~
10h；Diluted again with 120~140mL deionized water and 40~60mL hydrogen peroxide, above-mentioned gained dilute solution is put into
Is dialysed in analysis bag, obtain the solution that pH value is 6-7, then 12~20h, obtained carbonitride are dried under the conditions of being placed on 50~55 DEG C
(g-C3N4) nanometer sheet；
(3) preparation of carbonitrides/graphene composite material
(3-1) weigh graphene oxide that the step of 5mL concentration is 2~3mg/mL (1) obtain GO) solution is by graphite oxide
Carbonitride (the g-C that alkene (GO) solution is obtained with step (2)3N4) nanometer sheet in mass ratio be 5：3 ratio ultrasonic mixing is uniform,
(3-2) adds 80mL ethylenediamine, 95 DEG C of h of isothermal reaction 3 into the solution after above-mentioned ultrasonic mixing；
1mL CTAB solution is added in above-mentioned reacted solution by (3-3), after reaction 7h, is taken out product, is used deionization
Water washing 3-5 times；It is freeze-dried under the conditions of being placed on -50 DEG C after washing, obtains carbonitride/graphene composite wood of three-dimensional structure
Material.
Compared with prior art, the beneficial effect having is the present invention：
Carbonitride/graphene composite material of three-dimensional structure prepared by the present invention, is coupled due to adding ethylenediamine with CTAB,
Avoid reuniting in composite building-up process and can increase surface area, improve composite photocatalysis performance, while being easy to reclaim, side
Just control, it can be made to be applied in more broad range.
Carbonitride/graphene composite material of three-dimensional structure prepared by the present invention, can by adjust graphene oxide GO with
Carbonitride g-C3N4Content and its synthesis condition controlling organization performance, improve composite retractility.
A kind of preparation method of carbonitride/graphene of three-dimensional structure of the present invention, with low cost, technique is simple,
Advantage simple to operate, can be widely applied to industrial production manufacture.
Brief description of the drawings
Fig. 1 spreads out for a kind of x-ray powder of carbonitride/graphene composite material of three-dimensional structure of the embodiment of the present invention
It is to penetrate abscissa in (XRD) figure, Fig. 1 twice of the incident angle of x-ray, and unit is " angstrom ", 1 angstrom=0.1 nm, and ordinate is
Intensity after diffraction, unit is 1.
Fig. 2 is a kind of transmitted electron of carbonitride/graphene composite material of three-dimensional structure made from the embodiment of the present invention
Microscope (TEM) figure.
Fig. 3 is a kind of photocatalytic of carbonitride/graphene composite material of three-dimensional structure made from the embodiment of the present invention
Abscissa is light application time in energy curve map, Fig. 3, and unit is min, and ordinate is degradation rate, and unit is 1.
Embodiment
The present invention is expanded on further below by specific embodiment and with reference to accompanying drawing, but is not limited to the present invention.
Embodiment 1
The preparation method of carbonitride/graphene composite material of a kind of three-dimensional structure, it is characterised in that specifically comprising following step
Suddenly：
(1) prepares graphene oxide (GO) using Hummers methods；The graphene oxide solution of certain volume is taken, water is used
Concentration 3mg/ml is diluted to, 1h is stirred, obtains graphene oxide (GO) solution；
(2) preparation of carbonitrides (g-C3N4) nanometer sheet：
5 g dicyandiamide is put into Muffle furnace by (2-1) is warming up to 550 DEG C, is incubated 4 h, carbonitride (g-C is made3N4)；
(2-2) is by above-mentioned gained carbonitride (g-C3N4) add to 100mL concentrated sulfuric acid H2SO4In solution, stirred under agitator
Mix 24h；Then, under condition of ice bath, 1g sodium nitrate (NaNO is sequentially added3) and 10g potassium permanganate (KMnO4) stirring
10h；Diluted again with 140mL deionized water and 60mL hydrogen peroxide；Above-mentioned gained dilute solution is put into bag filter
Row dialysis, then 20h is dried under the conditions of 55 DEG C, carbonitride (g-C3N4) nanometer sheet is made；
(3) preparation of carbonitrides/graphene composite material：
(3-1) weigh 5mL concentration for 3mg/mL the step of (1) obtain graphene oxide GO) solution, by graphene oxide
GO) the obtained carbonitride (g-C of solution and step (2)3N4) nanometer sheet in mass ratio be 5：3 ratio ultrasonic mixing is uniform,
(3-2) adds 80mL ethylenediamine, 95 DEG C of h of isothermal reaction 3 into the solution after above-mentioned ultrasonic mixing；
1mL CTAB solution is added in above-mentioned reacted solution by (3-3), after reaction 7h, is taken out product, is used deionization
Water washing 3-5 times；It is freeze-dried under the conditions of being placed on -50 DEG C after washing, obtains carbonitride/graphene composite wood of three-dimensional structure
Material.
Carbonitride/graphene composite material obtained by this example is subjected to XRD spectrum measure, transmission electron microscope respectively
(TEM) determine and its photocatalysis performance is determined.Wherein figure l is the XRD of carbonitride/graphene composite material, it can be seen from figure 1 that
Carbonitride (g-C3N4) be supported on graphene oxide (GO)；Fig. 2 is the TEM figures of carbonitride/graphene composite material, can from Fig. 2
To find out, carbonitride (g-C3N4) be supported on graphene oxide (GO), it is uniformly dispersed；Fig. 3 is carbonitride/graphene composite wood
Carbonitride/graphene composite material is under the conditions of visible ray illumination 40min in the photocatalysis performance curve map of material, figure, 20ppm's
Methylene blue can degrade 90%, and composite has efficient photocatalysis performance.
Claims (1)
1. the preparation method of carbonitride/graphene composite material of a kind of three-dimensional structure, it is characterised in that this method includes following
Step：
（1）Graphene oxide (GO) is prepared using Hummers methods：The graphene oxide solution of certain volume is taken, it is dilute with water
1~5mg/ml of concentration is released, 0.5~2h is stirred, obtains graphene oxide (GO) solution；
（2）Carbonitride (g-C3N4）The preparation of nanometer sheet：
5~20g dicyandiamide is put into Muffle furnace by (2-1) is warming up to 550 DEG C, is incubated 2~4 h, carbonitride (g- is made
C3N4）；
(2-2) is by above-mentioned gained carbonitride (g-C3N4) add into 100mL concentrated sulfuric acid solution, stir 20 under agitator
~24h, then, under condition of ice bath, sequentially adds 1g sodium nitrate (NaNO3) and 10g potassium permanganate (KMnO4), stirring 8
~10h；Diluted again with 120~140mL deionized water and 40~60mL hydrogen peroxide, above-mentioned gained dilute solution is put into
Is dialysed in bag filter, obtain pH value and be 6-7 solution, then dry 12~20h under the conditions of being placed on 50~55 DEG C, be made and nitrogenize
Carbon (g-C3N4) nanometer sheet；
（3）The preparation of carbonitride/graphene composite material：
(3-1) weigh graphene oxide that the step of 5mL concentration is 2~3mg/mL (1) obtain GO) solution is by graphite oxide
Carbonitride (the g-C that alkene (GO) solution is obtained with step (2)3N4) nanometer sheet in mass ratio be 5：3 ratio ultrasonic mixing is uniform；
(3-2) adds 80mL ethylenediamine, 95 DEG C of h of isothermal reaction 3 into the solution after above-mentioned ultrasonic mixing；
1mL CTAB solution is added in above-mentioned reacted solution by (3-3), after reaction 7h, is taken out product, is used deionization
Water washing 3-5 times；It is freeze-dried under the conditions of being placed on -50 DEG C after washing, obtains carbonitride/graphene composite wood of three-dimensional structure
Material.
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Cited By (13)
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| CN108298523A (en) * | 2018-02-28 | 2018-07-20 | 中国科学院金属研究所 | A kind of graphene-based compound porous foam of the isotropism high resiliency of temperature-stable |
| CN108579789A (en) * | 2018-05-07 | 2018-09-28 | 常州大学 | A kind of preparation method for synthesizing ethylene carbonate process solid catalyst |
| CN109160498A (en) * | 2018-09-27 | 2019-01-08 | 景德镇陶瓷大学 | A kind of three-dimensional net structure class graphene carbonitride and its preparation method and application |
| 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 |
| 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 |
| CN110316724A (en) * | 2019-06-21 | 2019-10-11 | 浙江工商大学 | A kind of three-dimensional modified graphene aeroge and its preparation and the application in water process |
| CN110385146A (en) * | 2019-08-08 | 2019-10-29 | 上海大学 | A kind of Ni0.85Se/PDA/g-C3N4Composite photo-catalyst and its application |
| CN110433849A (en) * | 2019-08-23 | 2019-11-12 | 江南大学 | A kind of graphene oxide quantum dot/oxygen doping nitride porous carbon/graphene oxide ternary aerogels |
| CN110538672A (en) * | 2019-07-25 | 2019-12-06 | 广东工业大学 | Composite visible light response photocatalyst material and preparation method and application thereof |
| CN110804477A (en) * | 2019-11-25 | 2020-02-18 | 贵州明志典成科技有限公司 | Graphene engine oil antiwear agent and preparation method thereof |
| CN110980666A (en) * | 2019-12-04 | 2020-04-10 | 山西大学 | g-C3N4Nano thin sheet/graphene oxide composite material and preparation method and application thereof |
| CN113617351A (en) * | 2021-08-27 | 2021-11-09 | 西安理工大学 | Graphite-like phase carbon nitride/graphene oxide composite aerogel and method |
| CN115350720A (en) * | 2022-08-22 | 2022-11-18 | 桂林电子科技大学 | Heterojunction structure rGO/g-CN aerogel and preparation method and application thereof |
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