CN104108688A - Method for preparing carbon nitride nanoribbon and secondary assembly structure of carbon nitride nanoribbon - Google Patents

Method for preparing carbon nitride nanoribbon and secondary assembly structure of carbon nitride nanoribbon Download PDF

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CN104108688A
CN104108688A CN201410375765.3A CN201410375765A CN104108688A CN 104108688 A CN104108688 A CN 104108688A CN 201410375765 A CN201410375765 A CN 201410375765A CN 104108688 A CN104108688 A CN 104108688A
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carbon nano
preparation
azotized carbon
nano band
aqueous solution
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CN104108688B (en
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楚增勇
原博
李公义
蒋振华
胡天娇
王璟
李义和
王春华
王孝杰
王清华
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National University of Defense Technology
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Abstract

The invention discloses a method for preparing a carbon nitride nanoribbon and a secondary assembly structure of the carbon nitride nanoribbon. The method for preparing the carbon nitride nanoribbon comprises the following steps: (1) preparing materials; (2) heating; (3) separating; (4) drying. The invention also provides a method for preparing the secondary assembly structure of the carbon nitride nanoribbon. The method is simple in process and low in cost, and the used template is a sodium chloride crystal and can be easily dissolved and removed by water; the obtained nanoribbon is large in specific surface area, high in water solubility and good in stability, and the aqueous solution can be stabilized for over 15 days; moreover, according to the obtained nanoribbon, different secondary assembly structures, such as micro-ribbons, microrods, microtubes, bouquets and ball-flowers, are easily obtained by utilizing different alcohols, and the obtained higher structure has wider application in the fields of environment conservation, energy, national defense and chemical industry.

Description

The preparation method of a kind of azotized carbon nano band and secondary groups assembling structure thereof
Technical field
The present invention relates to the preparation method of a kind of azotized carbon nano band and secondary groups assembling structure thereof, particularly a kind of graphite-phase carbonitride (g-C for preparing 3n 4) method of nano belt and secondary groups assembling structure thereof.
Background technology
Carbonitride is elementary composition by carbon and two kinds, nitrogen, and element reserves are abundant, wide material sources, simple synthetic method, good economy performance and be easy to obtain.Graphite-phase carbonitride (g-C 3n 4) belonging to narrow gap semiconductor, its band gap width is about 2.7 eV, nontoxic, not containing metal.Meanwhile, g-C 3n 4also there is the strong and electron transfer rate advantages of higher of good mechanical property, thermostability, acid-alkali-corrosive-resisting (all thering is good stability the aqueous solution of pH from 0 to 14) and oxidation capacity.Based on above-mentioned advantage, g-C 3n 4can be used as a kind of novel visible light catalyst uses, can be applied in the reactions such as photochemical catalysis, electrocatalysis, organic oxygenation dehydrogenation, simultaneously at other field, as the storage of energy transformation, gas and catch, the aspect such as the purification of water pollutant, solar cell also applies well.
The preparation method that carbonitride is conventional mainly contains hot high pressure solution, vapour deposition process, ion implantation, hydro-thermal or solvent thermal synthesis method and electrochemical deposition method etc.In recent years, a kind of method of the organic matter precursors such as direct heating condensation polymerization cyanamide, cyanamid dimerization and trimeric cyanamide, becomes many preparation g-C of application in recent years 3n 4the method of crystal.But block materials specific surface area prepared by these methods is often less than 10 m 2/ g, practical ranges is limited.
For this reason, conventionally consider to introduce the adjustable pore structure in aperture in body phase carbon nitride, or nanometer particle size and the pattern of change carbonitride increase its specific surface area.2005, (" Preparation and characterization of well-ordered hexagonal mesoporous carbon nitride " the Adv Mater such as Vinu, 2005,17:1648) take mesoporous SBA-15 as hard template, prepare the carbonitride MCN-1 with order mesoporous structure, but porous g-C 3n 4after synthetic, hard template be need to remove, hypertoxic HF or NH often needed to use 4hF 2, larger to the injury of human body.Except vesicular structure, also can utilize space confinement method, synthetic carbonitride quantum dot that method, hot stripping method, solvent stripping method etc. prepare a series of different-shapes, nano wire, nanotube, nano belt, nanometer rod, nano particle, nanometer ball, the nano-cluster smashed (referring to " preparation and the application of high-specific surface area greying carbonitride ", petroleum journal, 2014,30:158).For example, (" Condensed graphitic carbon nitride nanorods by nanoconfinement:Promotion of crystallinity on photocatalytic conversion " the Chem Mater such as Li, 2011,23:4344) take anodised aluminium is presoma as template, nitrile amine, prepares the azotized carbon nano rod of high-crystallinity and photocatalysis performance by confinement thermal polycondensation; The people such as Yang (" Synthesis and characterization of nitrogen-rich carbon nitride nanobelts by pyrolysis of melamine " Appl Phys A, 2011,105:161) utilize trimeric cyanamide for presoma, at 700 ℃, 1000 ℃ two-step processes, obtained respectively the nano strip product of fiber pattern; The people such as Zhao (" Large-scale synthesis of nitrogen-rich carbon nitride microfibers by using graphitic carbon nitride as precursor " Adv Mater, 2008,20:1777) utilize carbonitride to prepare the macrofibers that diameter approaches micron being slowly warming up to 680 ℃ for presoma; (" the Synthesis and characterization of graphite-like carbon nitride nanobelts and nanotubes " Nanotechnology such as Li, 2007,18:1) take Dicyanodiamide and trimeric cyanamide as presoma, under 290 ℃, the condition of 4.5~5 MPa, obtained nano belt, nanotube-shaped product.
The preparation method of existing azotized carbon nano structure has all utilized the stability of ring texture carbonitride to a certain extent, or constructs nanostructure by template, or utilizes its distillation restructuring characteristic growth of nanostructures.But, in method for preparing template, as hard template silicon oxide, remove difficulty; In growth preparation method, the nanostructure of high growth temperature is difficult to carry out secondary assembling again, is difficult to construct more senior nanostructure.
Summary of the invention
The technical problem to be solved in the present invention is, overcomes the deficiencies in the prior art, the preparation method who provides a kind of template to remove easier azotized carbon nano band and secondary groups assembling structure thereof, and the nano belt assembling of gained is easier to.
The technical scheme that the present invention solves its technical problem employing is:
The preparation method of the present invention's azotized carbon nano band, comprises the following steps:
(1) get the raw materials ready: weigh in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are preferred 1:2~3 of 1:1~5(); Trimeric cyanamide and sodium chloride crystal are placed in to mortar, grind the preferred 15-20min of 10~30min() make mixture all by 400~600 orders (preferably 450-550 order) sieve;
(2) heating: the mixture that step (1) is sieved is placed in porcelain boat, be placed in tube furnace, with preferred 2 ~ 6 ml/min of 1~10ml/min(, more preferably the logical nitrogen of flow velocity 3-4 ml/min), with preferred 5 ~ 20 ℃/min of 1~30 ℃/min(, more preferably temperature rise rate 8-15 ℃/min) is raised to 400~700 ℃ (preferably 500 ~ 600 ℃) and is incubated 1~2h, with stove, is chilled to room temperature;
(3) separation: step (2) products therefrom is placed in to mortar, grinding 5~30min makes mixture all by 400~600 mesh sieve, be dissolved in again in deionized water, with the preferred 700-800 rpm of 500 ~ 1000rpm() centrifugation rate remove precipitation, use dialysis tubing dialysis 24~48h that molecular weight is 500~3000 to remove sodium-chlor, obtain the aqueous solution that contains nano belt;
(4) dry: by step (3) obtained aqueous solution at-40~-10 ℃ of preferred 20-30h of lyophilize 10~48h() to constant weight, obtain azotized carbon nano band.
The preparation method of the present invention's azotized carbon nano band secondary groups assembling structure, comprises the following steps:
(1) get the raw materials ready: weigh in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are 1:1~5; Trimeric cyanamide and sodium chloride crystal are placed in to mortar, grind 10~30min and make mixture all by 400~600 mesh sieve;
(2) heating: the mixture that step (1) is sieved is placed in porcelain boat, be placed in tube furnace, with preferred 3 ~ 6 ml/min of 1~10ml/min() the logical nitrogen of flow velocity, with preferred 5 ~ 20 ℃/min of 1~30 ℃/min() temperature rise rate be raised to 400~700 ℃ (preferably 500 ~ 600 ℃) and be incubated 1~2h, with stove, be chilled to room temperature;
(3) separation: step (2) products therefrom is placed in to mortar, grinding 5~30min makes mixture all by 400~600 mesh sieve, be dissolved in deionized water, centrifugation rate with 500 ~ 1000rpm is removed precipitation, use dialysis tubing dialysis 24~48h that molecular weight is 500~3000 to remove sodium-chlor, obtain the aqueous solution that contains nano belt;
(4) assembling is with dry: in step (3) obtained aqueous solution, drip the alkyl alcohol that is equivalent to 0.5~2 times of aqueous solution volume, be precipitated thing, throw out is placed in to baking oven, at 50~100 ℃ of dry 1~24h, to constant weight, can obtains carbonitride secondary groups assembling structure.
In step (4), a kind of in described alkyl alcohol particular methanol, ethanol, propyl alcohol, propyl carbinol, Virahol, 3-amylalcohol.  
Gained nanometer bandwidth of the present invention 80~120nm, its secondary groups assembling structure comprises micro belt, micron bar, micron tube, bouquet and bouquet.Use different alcohol, can obtain different secondary groups assembling structures: use methyl alcohol, ethanol, obtain micro belt; Use propyl alcohol, obtain bouquet; Use propyl carbinol, obtain bouquet; Use Virahol, obtain micron tube; Use 3-amylalcohol, obtain micron bar.
The present invention has following outstanding advantages:
(1) template of using is selected sodium chloride crystal, and technique is simpler, and cost is low, can by water dissolution, remove at an easy rate;
(2) high (90~160 m of nano belt specific surface area that obtain 2/ g), water-soluble very good, good stability, the aqueous solution can be stablized more than 15 days;
(3) nano belt obtaining utilizes different alcohol to obtain different secondary groups assembling structures at an easy rate, as micro belt, micron bar, micron tube, bouquet and bouquet;
(4) higher structure obtaining will have application more widely at environmental protection, the energy, national defence and chemical field.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 makes the scanning electron microscope (SEM) photograph of " nano belt ";
Fig. 2 is that the embodiment of the present invention 1 makes the transmission electron microscope picture of " nano belt ";
Fig. 3 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 10 makes secondary groups assembling structure " micro belt ";
Fig. 4 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 12 makes secondary groups assembling structure " bouquet ";
Fig. 5 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 14 makes secondary groups assembling structure " bouquet ";
Fig. 6 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 17 makes secondary groups assembling structure " micron tube ";
Fig. 7 is the scanning electron microscope (SEM) photograph that the embodiment of the present invention 19 makes secondary groups assembling structure " micron bar ".
Embodiment
Below with reference to Figure of description and specific embodiment, the present invention is described in further details.
[embodiment 1-9 is the embodiment of preparation nano belt]
embodiment 1
The preparation method of the azotized carbon nano band of the present embodiment, comprises the following steps:
(1) get the raw materials ready: weigh trimeric cyanamide 1g, sodium chloride crystal 3g(is that trimeric cyanamide and sodium chloride crystal mass ratio are 1:3), be placed in mortar, grind 15min and make mixture all by 500 mesh sieve;
(2) heating: the mixture that step (1) is sieved is placed in porcelain boat, is placed in tube furnace, with the logical nitrogen of the flow velocity of 4ml/min, is raised to 550 ℃ and be incubated 2h with the temperature rise rate of 10 ℃/min, with stove, is chilled to room temperature;
(3) separation: step (2) products therefrom is placed in to mortar, grinding 10min makes mixture all by 500 mesh sieve, be dissolved in 50ml deionized water, centrifugation rate with 800rpm is removed precipitation, use the dialysis tubing dialysis 30h that molecular weight is 1500 to remove sodium-chlor, obtain the 50ml aqueous solution that contains nano belt;
(4) dry: by step (3) obtained aqueous solution at-30 ℃ of lyophilize 24h to constant weight, can obtain azotized carbon nano band.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 120m 2/ g, productive rate is 86wt%.Its scanning electron microscope (SEM) photograph as shown in Figure 1; Its transmission electron microscope picture as shown in Figure 2.
embodiment 2
Only be with the difference of embodiment 1, in the present embodiment, trimeric cyanamide and sodium chloride crystal mass ratio are 1:1, in step (1), weigh trimeric cyanamide 1g, sodium chloride crystal 1g, and all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 90m 2/ g, productive rate is 60wt%.
embodiment 3
Only be with the difference of embodiment 1, in the present embodiment, trimeric cyanamide and sodium chloride crystal mass ratio are 1:5, in step (1), weigh trimeric cyanamide 1g, sodium chloride crystal 5g, and all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 105m 2/ g, productive rate is 73wt%.
embodiment 4
Only be with the difference of embodiment 1, in the present embodiment, in step (1), step (3), all by 400 mesh sieve, all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~110nm, specific surface area is 114m 2/ g, productive rate is 80wt%.
embodiment 5
Only be with the difference of embodiment 1, in the present embodiment, in step (1), step (3), all by 600 mesh sieve, all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 80~100nm, specific surface area is 118m 2/ g, productive rate is 76wt%.
embodiment 6
Only be with the difference of embodiment 1, in the present embodiment, step (2) is with the logical nitrogen of the flow velocity of 10ml/min, with the temperature rise rate of 30 ℃/min, is raised to 700 ℃ and be incubated 1h, and all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 95m 2/ g, productive rate is 50wt%.
 
embodiment 7
Only be with the difference of embodiment 1, in the present embodiment, step (2) is with the logical nitrogen of the flow velocity of 1ml/min, with the temperature rise rate of 1 ℃/min, is raised to 400 ℃ and be incubated 2h, and all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 101m 2/ g, productive rate is 70wt%.
embodiment 8
Only be with the difference of embodiment 1, in the present embodiment, step (3) is removed precipitation with the centrifugation rate of 1000rpm, uses the dialysis tubing dialysis 48h that molecular weight is 3000 to remove sodium-chlor, and all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 90~100nm, specific surface area is 110m 2/ g, productive rate is 45wt%.
embodiment 9
Only be with the difference of embodiment 1, in the present embodiment, step (3) is removed precipitation with the centrifugation rate of 500rpm,, use the dialysis tubing dialysis 24h that molecular weight is 500 to remove sodium-chlor, all the other are identical with embodiment 1.
The present embodiment gained azotized carbon nano bandwidth 100~120nm, specific surface area is 99m 2/ g, productive rate is 89wt%.
[embodiment 10-19 is the embodiment of preparation secondary groups assembling structure]
embodiment 10
The preparation method of the carbonitride micro belt of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 1 step (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip methyl alcohol 50ml, be precipitated thing, throw out is placed in to baking oven, at 70 ℃ of dry 12h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micro belt, wide 0.5~1.0mm.Its scanning electron microscope (SEM) photograph as shown in Figure 3.
 
embodiment 11
The preparation method of the carbonitride micro belt of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 2 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: to step (3) the gained 50ml aqueous solution, drip ethanol 25ml, be precipitated thing, throw out is placed in to baking oven, at 50 ℃ of dry 24h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micro belt, wide 0.6~1.1mm.
embodiment 12
The preparation method of the carbonitride bouquet of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 3 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip propyl alcohol 75ml, be precipitated thing, throw out is placed in to baking oven, at 100 ℃ of dry 1h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is bouquet, corolla diameter 5.0~20.0mm.Its scanning electron microscope (SEM) photograph as shown in Figure 4.
 
embodiment 13
Only be with the difference of embodiment 10, in step (4), in step (3) the gained 50ml aqueous solution, drip propyl alcohol 100ml, all the other are identical with embodiment 10.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is bouquet, corolla diameter 4.0~24.0mm.
embodiment 14
The preparation method of the carbonitride bouquet of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 5 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: to step (3) the gained 50ml aqueous solution, drip propyl carbinol 75ml, be precipitated thing, throw out is placed in to baking oven, at 90 ℃ of dry 10h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is bouquet, bouquet diameter 30.0~50.0mm.Its scanning electron microscope (SEM) photograph is as shown in Figure 5.
embodiment 15
Only be with the difference of embodiment 10, in step (4), in step (3) the gained 50ml aqueous solution, drip propyl carbinol 65ml, all the other are identical with embodiment 10.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is bouquet, bouquet diameter 35.0~45.0mm.
embodiment 16
The preparation method of the carbonitride bouquet of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 7 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip propyl carbinol 80ml, be precipitated thing, throw out is placed in to baking oven, at 60 ℃ of dry 20h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is bouquet, bouquet diameter 30.0~40.0mm.
 
embodiment 17
Only be with the difference of embodiment 10, in step (4), in step (3) the gained 50ml aqueous solution, drip Virahol 40ml, other are identical with embodiment 10.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micron tube, diameter 3.0~5.0mm.Its scanning electron microscope (SEM) photograph as shown in Figure 6.
 
embodiment 18
The preparation method of the present invention's carbonitride micron tube, comprises the following steps:
Step (1), (2), (3) and embodiment 6 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip Virahol 80ml, be precipitated thing, throw out is placed in to baking oven, at 90 ℃ of dry 2h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micron tube, diameter 3.0~4.5mm.
 
embodiment 19
The preparation method of the carbonitride micron bar of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 9 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip 3-amylalcohol 30ml, be precipitated thing, throw out is placed in to baking oven, at 80 ℃ of dry 5h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micron bar, diameter 0.5~2.0mm.Its scanning electron microscope (SEM) photograph as shown in Figure 7.
 
embodiment 20
The preparation method of the carbonitride micron bar of the present embodiment, comprises the following steps:
Step (1), (2), (3) and embodiment 9 steps (1), (2), (3) are identical.
Step (4) assembling is with dry: in step (3) the gained 50ml aqueous solution, drip 3-amylalcohol 70ml, be precipitated thing, throw out is placed in to baking oven, at 100 ℃ of dry 1h to constant weight.
The present embodiment gained azotized carbon nano band secondary groups assembling structure is micron bar, diameter 0.5~1.5mm.
Below be only the preferred embodiment of the present invention, protection scope of the present invention is also not only confined to above-described embodiment, conceives various process programs without substantial differences all in protection scope of the present invention with the present invention.

Claims (10)

1. a preparation method for azotized carbon nano band, is characterized in that, comprises the following steps:
(1) get the raw materials ready: weigh in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are 1:1~5; Trimeric cyanamide and sodium chloride crystal are placed in to mortar, grind 10~30min and make mixture all by 400~600 mesh sieve;
(2) heating: the mixture that step (1) is sieved is placed in porcelain boat, is placed in tube furnace, with the logical nitrogen of the flow velocity of 1~10ml/min, is raised to 400~700 ℃ and be incubated 1~2h with the temperature rise rate of 1~30 ℃/min, with stove, is chilled to room temperature;
(3) separation: step (2) products therefrom is placed in to mortar, grinding 5~30min makes mixture all by 400~600 mesh sieve, be dissolved in again in deionized water, centrifugation rate with 500 ~ 1000rpm is removed precipitation, use dialysis tubing dialysis 24~48h that molecular weight is 500~3000 to remove sodium-chlor, obtain the aqueous solution that contains nano belt;
(4) dry: by step (3) obtained aqueous solution at-40~-10 ℃ of lyophilize 10~48h to constant weight, obtain azotized carbon nano band.
2. the preparation method of azotized carbon nano band according to claim 1, is characterized in that, in step (2), the flow velocity that passes into nitrogen is 2 ~ 6 ml/min.
3. the preparation method of azotized carbon nano band according to claim 1 and 2, is characterized in that, in step (2), temperature rise rate is 5 ~ 20 ℃/min.
4. the preparation method of azotized carbon nano band according to claim 1 and 2, is characterized in that, in step (2), is warmed up to 500 ~ 600 ℃.
5. the preparation method of the secondary groups assembling structure of azotized carbon nano band as prepared in claim 1-4, is characterized in that, comprises the following steps:
(1) get the raw materials ready: weigh in proportion trimeric cyanamide and sodium chloride crystal, wherein trimeric cyanamide and sodium chloride crystal mass ratio are 1:1~5; Trimeric cyanamide and sodium chloride crystal are placed in to mortar, grind 10~30min and make mixture all by 400~600 mesh sieve;
(2) heating: the mixture that step (1) is sieved is placed in porcelain boat, is placed in tube furnace, with the logical nitrogen of the flow velocity of 1~10ml/min, is raised to 400~700 ℃ and be incubated 1~2h with the temperature rise rate of 1~30 ℃/min, with stove, is chilled to room temperature;
(3) separation: step (2) products therefrom is placed in to mortar, grinding 5~30min makes mixture all by 400~600 mesh sieve, be dissolved in deionized water, centrifugation rate with 500 ~ 1000rpm is removed precipitation, use dialysis tubing dialysis 24~48h that molecular weight is 500~3000 to remove sodium-chlor, obtain the aqueous solution that contains nano belt;
(4) assembling is with dry: in step (3) obtained aqueous solution, drip the alkyl alcohol that is equivalent to 0.5~2 times of aqueous solution volume, be precipitated thing, throw out is placed in to baking oven, at 50~100 ℃ of dry 1~24h, to constant weight, obtain carbonitride secondary groups assembling structure.
6. the preparation method of azotized carbon nano band secondary groups assembling structure according to claim 5, is characterized in that, in step (4), described alkyl alcohol is a kind of in methyl alcohol, ethanol, propyl alcohol, propyl carbinol, Virahol, 3-amylalcohol.
7. according to the preparation method of the azotized carbon nano band secondary groups assembling structure described in claim 5 or 6, it is characterized in that, use different alcohol, obtain different secondary groups assembling structures: use methyl alcohol, ethanol, obtain micro belt; Use propyl alcohol, obtain bouquet; Use propyl carbinol, obtain bouquet; Use Virahol, obtain micron tube; Use 3-amylalcohol, obtain micron bar.
8. according to the preparation method of the azotized carbon nano band described in claim 5 or 6, it is characterized in that, in step (2), the flow velocity that passes into nitrogen is 3 ~ 6 ml/min.
9. according to the preparation method of the azotized carbon nano band described in claim 5 or 6, it is characterized in that, in step (2), temperature rise rate is 5 ~ 20 ℃/min.
10. according to the preparation method of the azotized carbon nano band described in claim 5 or 6, it is characterized in that, in step (2), be warmed up to 500 ~ 600 ℃.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102992282A (en) * 2012-11-08 2013-03-27 南京大学 Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102992282A (en) * 2012-11-08 2013-03-27 南京大学 Mesoporous C3N4 photocatalytic material prepared by using molten salt method and application thereof in photocatalysis field

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MICHAEL J. BOJDYS,ET AL.: "Ionothermal Synthesis of Crystalline, Condensed, Graphitic Carbon Nitride", 《CHEM. EUR. J》 *

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