CN106744745B - A kind of graphite phase carbon nitride nanotube and preparation method thereof of carbon doping - Google Patents
A kind of graphite phase carbon nitride nanotube and preparation method thereof of carbon doping Download PDFInfo
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Abstract
The invention discloses a kind of graphite phase carbon nitride nanotube and preparation method thereof of carbon doping, preparation process are as follows: melamine is dispersed in the ethanol solution of TSL 8330 first, centrifugal drying obtains solid powder after hydro-thermal reaction；(3- mercaptopropyi) trimethyl oxosilane is mixed evenly with ethyl orthosilicate, the mixed solution that second alcohol and water is added is again stirring for, the SiO of centrifuge separation MPS modification2Solution.The solid powder of pretreated melamine is added to the SiO of MPS modification2It in solution, is centrifuged after stirring, is dry, calcined to obtain product, product is performed etching by HF solution to obtain the final product.Preparation process of the present invention is novel, convenient, controllability is strong, resulting nanotube has size more uniform, the advantages that tube wall is relatively thin, electric conductivity is preferable, photocatalysis property is excellent, it can be used for constructing a variety of heterojunction structures, have good application potential in terms of photocatalysis degradation organic contaminant, photodissociation aquatic products.
Description
Technical field
The present invention relates to a kind of graphite phase carbon nitride nanotubes and preparation method thereof of carbon doping, belong to semiconductor material
Doping vario-property preparation technical field.
Background technique
Single similar graphitization carbonitride (g-C3N4) it is used as a kind of organic polymer semiconductor, due to its good physics and chemistry
Property, easily preparation, be stabilized in air, forbidden bandwidth is that 2.7eV such as can be excited at the advantages in visible-range, make it
As a kind of novel organic photochemical catalyst, it can be used for photodissociation aquatic products hydrogen and produce oxygen, degradable organic pollutant, hydrogen storage etc., thus
It can be widely used in many fields such as environment, the energy, biology.
However, due to the body phase g-C of simple high temperature polymerization preparation3N4Layer it is poor with interlayer electric conductivity, make its light induced electron and
Hole-recombination rate is higher, and photocatalytic activity is poor.People are frequently with method optimizings such as doping, nano modification, building heterojunction structures
Its performance.Pass through numerous studies, ion doping g-C3N4Nano material also has made great progress.But the g-C after doping3N4
There are still the regulation of pattern difficulty, difficult preparation, pattern is single the deficiencies of, by the method report of doping regulation carbonitride pattern compared with
It is few.
Summary of the invention
The present invention is directed to g-C3N4The single shortcoming of the pattern of doping vario-property provides a kind of carbon doped graphite and mutually nitrogenizes
The preparation method of carbon nanotube, this method simple process, the carbonitride pattern after resulting doping is special, is nanotube, tube wall
It is relatively thin, crystallinity is good, surface defect is less.
Specific technical solution of the present invention is as follows:
The present invention provides a kind of graphite phase carbon nitride nanotube of carbon doping, the graphite phase carbon nitride shape of the carbon doping
Looks are hollow nanotube, and nanotube is crimped by nanometer sheet, and thickness of pipe wall 10nm-15nm, nanotube length is less than 1 μ
M, diameter dimension are 95-200 nm.
The present invention also provides a kind of preparation methods of the graphite phase carbon nitride nanotube of carbon doping, comprising the following steps:
(1) it in a kettle disperses melamine in the ethanol solution of TSL 8330, high-temperature water
After thermal response, centrifuge separation is dried to obtain solid powder；
(2) (3- mercaptopropyi) trimethyl oxosilane will be added in ethyl orthosilicate, stirring obtains homogeneous solution A；
(3) ethyl alcohol, water are mixed and stirred for, obtain solution B；
(4) solution A is added in solution B, stirring after a certain period of time, is centrifugally separating to obtain precipitating；
(5) precipitating that step (4) obtains is dispersed in water again, the solid powder that step (1) obtains then is added, stirs
It is dry after being centrifuged, being washed after mixing uniformly, white solid powder is obtained, white solid powder is placed in quartz boat in inertia
It is calcined under gas shield, obtains product；
(6) carbon doping is obtained through centrifuge washing, drying with the product obtained after the calcining of the HF solution etches of high concentration
Azotized carbon nano pipe.
Further, in step (1), the melamine is dense in the ethanol solution of TSL 8330
Degree is 0.015~0.019g/mL；The volume ratio of the TSL 8330 and ethyl alcohol is 0.1 × 10-4~2.5 ×
10-4。
Further, in step (1), above-mentioned hydro-thermal reaction is to react for 24 hours under the conditions of 200-220 DEG C of temperature.
Further, in step (2), the volume ratio of the ethyl orthosilicate and (3- mercaptopropyi) trimethyl oxosilane is
100~250:1, the mixing time are 2h.
Further, in step (3), the ratio of the ethyl alcohol and water is 10:1 ~ 2, and the time of the stirring is 30min.
Further, in step (4), the volume ratio of the solution A and solution B is 1:108 ~ 118, and the ratio of optimization is 1:
113 ~ 115, the time of the stirring is 6-8h.
Further, in step (5), the solid powder that the step (1) obtains is 1.2 with the mass ratio of ethyl orthosilicate
~ 3.3, the time of the stirring is for 24 hours.
Further, in step (5), the calcining is to react 2 after being warming up to 560 °C -600 °C under the protection of nitrogen
Hour.
Further, in step (6), the mass fraction of the hydrofluoric acid solution is the % of 20 % ~ 40, etch period 24-
48h。
The present invention is using the method for auto-dope in numerous g-C3N4In doping be also it is very meaningful, it avoid impurity from
The introducing of son, the method for directlying adopt carbon atom doping, the substitution of C make the carbon atom and g-C of doping3N4Shape between heterocycle in structure
At delocalized pi-bond, the ratio for improving carbon and nitrogen-atoms promotes the migration of light induced electron to improve electric conductivity.
Appearance of nano material of the invention is the azotized carbon nano pipe of carbon doping, and tube wall is relatively thin, and preparation process is to presoma
It is pre-processed, mercapto-modified silica is recycled to make matrix template, first obtain presoma/SiO2Material, then use hydrogen
Fluoric acid etches template, and the azotized carbon nano pipe of carbon doping can be obtained in removal silica, is enriching graphitization carbonitride
Carbon doping vario-property also is carried out to it while pattern, meaning is larger in terms of material modification and topography optimization.The present invention is better than
The single product of the pattern of other element doping carbonitrides, new technology is simple, and cost is relatively low, and method can be used for preparing other
The doping vario-property of substance, with good application prospect.
Detailed description of the invention
The C-g-C that Fig. 1 embodiment of the present invention 1 synthesizes3N4X-ray diffraction (XRD) map of nanotube.
The C-g-C that Fig. 2 embodiment of the present invention 1 synthesizes3N4Scanning electron microscope (SEM) photo of nanotube.
The C-g-C that Fig. 3 embodiment of the present invention 1 synthesizes3N4The curve of photocatalytic degradation RhB under nanotube visible light.
The C-g-C that Fig. 4 embodiment of the present invention 2 synthesizes3N4Scanning electron microscope (SEM) photo of nanotube.
The C-g-C that Fig. 5 embodiment of the present invention 3 synthesizes3N4Scanning electron microscope (SEM) photo of nanotube.
The g-C that Fig. 6 comparative example 1 of the present invention synthesizes3N4Scanning electron microscope (SEM) photo.
The C-g-C that Fig. 7 comparative example 2 of the present invention synthesizes3N4Scanning electron microscope (SEM) photo of nano material.
The C-g-C that Fig. 8 comparative example 2 of the present invention synthesizes3N4The curve of photocatalytic degradation RhB under nano material visible light.
Specific embodiment
Below by embodiment, the present invention will be further elaborated, it should be appreciated that, following the description merely to
It explains the present invention, its content is not defined.
Embodiment 1
1.1 with volume be that 0.75g melamine is dispersed in containing 8 μ L aminopropyl trimethoxies in the reaction kettle of 100mL
In the 80ml ethanol solution of silane (APS), at 200 DEG C hydro-thermal for 24 hours after, centrifuge separation be dried to obtain solid powder；
1.2 are added 2 μ L(3- mercaptopropyis in 0.5mL ethyl orthosilicate (TEOS)) trimethyl oxosilane (MPS)
Solution stirs evenly, and obtains homogeneous solution A；
1.3 are mixed and stirred for 50mL ethyl alcohol, 5mL water uniformly, to obtain solution B；
1.4 the solution A that step 1.2 obtains is added in the solution B that step 1.3 obtains, and after stirring 6h, is centrifugally separating to obtain
Precipitating；
1.5 precipitatings for obtaining step 1.4 are dispersed again in 30mL water, and 1.1 steps of multiplicating are then added and obtain
1.2g treated melamine solid powder, it is after mixing evenly, dry after being centrifuged, being washed, obtain white solid powder
Powder is placed in quartz boat 580 DEG C of calcining 2h in nitrogen by end, and heating rate is 5 DEG C/min, obtains product；
1.6 be 40% with mass fraction HF solution etches step (5) in after calcining obtained product, etch period be
For 24 hours, through centrifuge washing, drying, the azotized carbon nano pipe of carbon doping is obtained.
Fig. 1 is the carbonitride of carbon doping and the g-C undoped with carbon3N4The X ray diffracting spectrum of sample, can from figure
Out, products obtained therefrom is graphite type carbon nitride, and (002) characteristic peak is compared to pure g-C3N4It deviates to the right.Fig. 2 is the sample after being etched
The stereoscan photograph of product, as can be seen from the figure nanotube carbonitride length dimension is 1 μm, and nanotube is hollow structure, by
Nanometer sheet crimps, and diameter is the nm of 95 nm ~ 200, thickness of pipe wall 10-15nm.Fig. 3 is that the graphite phase carbon nitride of carbon doping exists
The curve of photocatalytic degradation RhB under visible light.
Embodiment 2
2.1 with volume be that 1.2g melamine is dispersed in the 80ml ethyl alcohol containing 20 μ L APS in the reaction kettle of 100mL is molten
In liquid, at 220 DEG C hydro-thermal for 24 hours after, centrifuge separation be dried to obtain solid powder；
2.2 are added 5 μ L(3- mercaptopropyis in 0.5mL ethyl orthosilicate (TEOS)) trimethyl oxosilane (MPS)
Solution stirs evenly, and obtains homogeneous solution A；
2.3 are mixed and stirred for 50mL ethyl alcohol, 10mL water uniformly, to obtain solution B；
2.4 the solution A that step 1.2 obtains is added in the solution B that step 1.3 obtains, and after stirring 6h, is centrifugally separating to obtain
Precipitating；
2.5 precipitatings for obtaining step 1.4 are dispersed again in 30mL water, and 2.1 steps of multiplicating are then added and obtain
1.5g treated melamine solid powder, it is after mixing evenly, dry after being centrifuged, being washed, obtain white solid powder
Powder is placed in quartz boat 600 DEG C of calcining 2h in nitrogen by end, and heating rate is 5 DEG C/min, obtains product；
2.6 burnt with the HF solution etches step 3.5 that mass fraction is 40% after obtained product, etch period be 36 through from
Heart washing, drying, obtain the azotized carbon nano pipe of carbon doping.
Fig. 4 is the stereoscan photograph of the sample after being etched, as can be seen from the figure nanotube carbonitride length dimension
It is 1 μm, nanotube is hollow structure, is crimped by nanometer sheet, and diameter is the nm of 100 nm ~ 200, and thickness of pipe wall is 10-15 nm.
Embodiment 3
3.1 with volume be that 1.5g melamine is dispersed in the 80ml ethyl alcohol containing 10 μ L APS in the reaction kettle of 100mL is molten
In liquid, at 200 DEG C hydro-thermal for 24 hours after, centrifuge separation be dried to obtain solid powder；
3.2 10 μ L(3- mercaptopropyis are added in the 1mL ethyl orthosilicate (TEOS)) trimethyl oxosilane (MPS) is molten
Liquid stirs evenly, and obtains homogeneous solution A；
3.3 are mixed and stirred for 100mL ethyl alcohol, 12mL water uniformly, to obtain solution B；
3.4 the solution A that step 1.2 obtains is added in the solution B that step 1.3 obtains, and after stirring 6h, is centrifugally separating to obtain
Precipitating；
3.5 precipitatings for obtaining step 1.4 are dispersed again in 50mL water, and 2.1 steps of multiplicating are then added and obtain
1.4g treated melamine solid powder, it is after mixing evenly, dry after being centrifuged, being washed, obtain white solid powder
Powder is placed in quartz boat 560 DEG C of calcining 2h in nitrogen by end, and heating rate is 5 DEG C/min, obtains product；
3.6 burnt with the HF solution etches step 3.5 that mass fraction is 20% after obtained product, etch period 48h, warp
Centrifuge washing, drying obtain the azotized carbon nano pipe of carbon doping.
Fig. 5 is the stereoscan photograph of the sample after being etched, as can be seen from the figure the azotized carbon nano pipe of carbon doping
Length dimension is 1 μm, and nanotube is hollow structure, is crimped by nanometer sheet, and diameter is the nm of 95 nm ~ 200, and thickness of pipe wall is
10-15 nm。
Embodiment 4
The preparation method is the same as that of Example 1, unlike: MPS additional amount is 5 μ L, and the azotized carbon nano of gained carbon doping is tubular
Looks are same as Example 1, and for nanotube length having a size of 1 μm, nanotube is hollow structure, crimped by nanometer sheet, diameter is
The nm of 95 nm ~ 200, thickness of pipe wall are 10-15 nm.
Embodiment 5
Preparation method with embodiment 2, unlike: be 210 DEG C in melamine pretreatment hydrothermal temperature；Etching concentration is
20 % hydrofluoric acid solutions, etch period 30h, product morphology is same as Example 2, the azotized carbon nano length of tube of carbon doping
Having a size of 1 μm, nanotube is hollow structure, is crimped by nanometer sheet, and diameter is the nm of 95 nm ~ 200, thickness of pipe wall 10-15
nm。
Embodiment 6
Preparation method is with unlike embodiment 3: calcination temperature is 600 DEG C；HF etch period is 40h, products therefrom shape
Looks are identical with embodiment 3, and nanotube is hollow structure, crimped by nanometer sheet, the azotized carbon nano length of tube ruler of carbon doping
Very little is 1 μm, and diameter is the nm of 95 nm ~ 200, and thickness of pipe wall is 10-15 nm.
Comparative example 1
1.1 are added 2 μ L(3- mercaptopropyis in 0.5mL ethyl orthosilicate (TEOS)) trimethyl oxosilane (MPS)
Solution stirs evenly, and obtains homogeneous solution A；
1.2 are mixed and stirred for 50mL ethyl alcohol, 5mL water uniformly, to obtain solution B；
1.3 the solution A that step 1.1 obtains is added in the solution B that step 1.2 obtains, and after stirring 6h, is centrifugally separating to obtain
Precipitating；
1.4 precipitatings for obtaining step 1.4 are dispersed again in 30mL water, and 1.2g melamine is then added, and stirring is equal
It is dry after being centrifuged, being washed after even, white solid powder is obtained, powder is placed in quartz boat 580 DEG C of calcinings in nitrogen
2h, heating rate are 5 DEG C/min, obtain product；
1.5 be 40% with mass fraction HF solution etches step (5) in after calcining obtained product, etch period be
For 24 hours, through centrifuge washing, drying；
Gained sample topography is loose porous layer structure, does not obtain nanotube, and product is undoped pure stone
Black phase carbon nitride, as shown in Figure 6.
Comparative example 2
9.1 with volume be that 1.2g melamine is dispersed in 80ml ethyl alcohol in the reaction kettle of 100mL, hydro-thermal at 200 DEG C
After for 24 hours, centrifuge separation is dried to obtain solid powder；
9.2 are added 2 μ L(3- mercaptopropyis in 0.5mL ethyl orthosilicate (TEOS)) trimethyl oxosilane (MPS)
Solution stirs evenly, and obtains homogeneous solution A；
9.3 are mixed and stirred for 50mL ethyl alcohol, 20mL water uniformly, to obtain solution B；
9.4 the solution A that step 1.2 obtains is added in the solution B that step (3) obtain, and after stirring 6h, is centrifugally separating to obtain
Precipitating；
9.5 precipitatings for obtaining step 1.4 are dispersed again in 50mL water, and 9.1 steps of multiplicating are then added and obtain
1.5g treated melamine, it is after mixing evenly, dry after being centrifuged, being washed, obtain white solid powder, powder set
500 DEG C of calcining 2h, heating rate are 5 DEG C/min in nitrogen in quartz boat, obtain product；
9..6 the product that the HF solution etches step 3.5 for being 20% with mass fraction obtains after burning, etch period are warp for 24 hours
Centrifuge washing, drying obtain the carbonitride of carbon doping.
Fig. 7 is the stereoscan photograph of product, is random pattern, and Fig. 8 is the song of product Photocatalytic Activity for Degradation RhB
Line.As can be seen from the figure the carbonitride of carbon doping does not form the pattern of nanotube, and its photocatalytic activity is also adulterated than carbon
Azotized carbon nano pipe poor activity.
Claims (7)
1. a kind of preparation method of the graphite phase carbon nitride nanotube of carbon doping, which comprises the following steps:
(1) it in a kettle disperses melamine in the ethanol solution of TSL 8330, high temperature hydro-thermal is anti-
Ying Hou, centrifuge separation are dried to obtain solid powder；
(2) (3- mercaptopropyi) trimethoxy silane will be added in ethyl orthosilicate, stirring obtains homogeneous solution A；
(3) ethyl alcohol, water are mixed and stirred for, obtain solution B；
The ratio of the ethyl alcohol and water is 10:1 ~ 2, and the time of the stirring is 30min；
(4) solution A is added in solution B, stirring after a certain period of time, is centrifugally separating to obtain precipitating；
(5) precipitating that step (4) obtains is dispersed in water again, the solid powder that step (1) obtains then is added, stirring is equal
It is dry after being centrifuged, being washed after even, white solid powder is obtained, white solid powder is placed in quartz boat in inert gas
The lower calcining of protection, obtains product；
(6) nitridation of carbon doping is obtained through centrifuge washing, drying with the product obtained after the calcining of the HF solution etches of high concentration
Carbon nanotube；
The graphite phase carbon nitride pattern of the carbon doping is hollow nanotube, and nanotube is crimped by nanometer sheet, tube wall
Thickness is 10nm-15nm, and for nanotube length less than 1 μm, diameter dimension is 95-200 nm；
In step (1), concentration of the melamine in the ethanol solution of TSL 8330 be 0.015~
0.019g/mL；The volume ratio of the TSL 8330 and ethyl alcohol is 0.1 × 10-4~2.5 × 10-4；
In step (2), the volume ratio of the ethyl orthosilicate and (3- mercaptopropyi) trimethoxy silane is 100~250:1, institute
Stating mixing time is 2h.
2. preparation method according to claim 1, which is characterized in that in step (1), the hydro-thermal reaction is in temperature
It is reacted for 24 hours under the conditions of 200-220 DEG C.
3. preparation method according to claim 1, which is characterized in that in step (4), the volume of the solution A and solution B
Than being 6-8h for the time of 1:108 ~ 118, the stirring.
4. preparation method according to claim 3, which is characterized in that the volume ratio of the solution A and solution B be 1:113 ~
115。
5. preparation method according to claim 1, which is characterized in that in step (5), solid that the step (1) obtains
Powder is 1.2 ~ 3.3 with the mass ratio of ethyl orthosilicate, and the time of the stirring is for 24 hours.
6. preparation method according to claim 1, which is characterized in that in step (5), the calcining is in the protection of nitrogen
Under, it is reacted 2 hours after being warming up to 560 °C -600 °C.
7. preparation method according to claim 1, which is characterized in that in step (6), the mass fraction of the HF solution is
20 % ~ 40 %, etch period 24-48h.
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| CN108686691A (en) * | 2018-03-26 | 2018-10-23 | 南昌航空大学 | A kind of preparation method of Gd2 O3 class graphite phase carbon nitride catalysis material |
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| CN105217584A (en) * | 2015-10-12 | 2016-01-06 | 济南大学 | A kind of preparation method of azotized carbon nano pipe |
| CN105350113A (en) * | 2015-12-10 | 2016-02-24 | 济南大学 | Preparation method of nitride carbon nanofibers and obtained product |
| CN106179444A (en) * | 2016-06-29 | 2016-12-07 | 陶雪芬 | A kind of preparation method of activated carbon supported carbon doping graphite phase carbon nitride |
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| CN105217584A (en) * | 2015-10-12 | 2016-01-06 | 济南大学 | A kind of preparation method of azotized carbon nano pipe |
| CN105350113A (en) * | 2015-12-10 | 2016-02-24 | 济南大学 | Preparation method of nitride carbon nanofibers and obtained product |
| CN106179444A (en) * | 2016-06-29 | 2016-12-07 | 陶雪芬 | A kind of preparation method of activated carbon supported carbon doping graphite phase carbon nitride |
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