CN109603697A - A kind of nano-sized carbon mixes aeroge and its preparation method and application - Google Patents
A kind of nano-sized carbon mixes aeroge and its preparation method and application Download PDFInfo
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- CN109603697A CN109603697A CN201811582411.0A CN201811582411A CN109603697A CN 109603697 A CN109603697 A CN 109603697A CN 201811582411 A CN201811582411 A CN 201811582411A CN 109603697 A CN109603697 A CN 109603697A
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Abstract
The present invention provides the preparation methods that a kind of nano-sized carbon mixes aeroge, belong to aeroge technical field.The present invention mixes FL-CNs and conductive nanometer carbon material (carbon nanotube), and the ultralight nano-sized carbon for preparing three-dimensional porous high conductivity mixes aeroge, and aeroge obtained can be used as the electrode of high conductivity energy storage device in terms of electrochemical energy storage；In terms of catalysis characteristics, both it can be used directly as catalyst, function dough or loading functional nanoparticle can be passed through again, as catalyst carrier, effectively improve catalytic action, due to high-specific surface area and high nitrogen active site, so that the material high catalytic efficiency, can be effectively reduced the dosage of noble metal catalyst；Meanwhile being also used to high-end heat-insulation and heat-preservation system etc..
Description
Technical field
The invention belongs to aeroge preparation technical fields more particularly to a kind of nano-sized carbon to mix aeroge and preparation method thereof
And application.
Background technique
So-called nitrogen carbide refers to graphite-phase nitrogen carbide (g-CN), it is made of nitrogen, carbon, nitrogen and carbon atomic ratio > 1
The two-dimensional slice shaped polymer semiconductor material of class graphene-structured.There are hole in this material layer, structure was both different from
The graphene of complete carbon-coating structure, also different from nitrogen-doped graphene.Nitrogen carbide has adjustable band gap and excellent light absorption
The difference of performance, carbon and nitrogen chemical valence state, which causes to be carbonized, forms hole in nitrogen layer, and the nitrogen lone pair electrons that are arranged in hole or
NH functional group, can cause master/object cross reaction, and nitrogen carbide has wide in fields such as charge storage, ion diffusion, photocatalysis
General application prospect.
Since the nitrogen carbide nanoscale twins (FL-CNs) of single layer or few layer have photocatalysis performance outstanding, become a kind of
Emerging two-dimensional layer material.Two-dimensional layer material obtained has that photocatalysis performance is low in the prior art.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of nano-sized carbons to mix aeroge and its preparation method and application.
Nano-sized carbon made from preparation method provided by the invention mixes aeroge with three-dimensional net structure, and catalytic performance is excellent.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides the preparation methods that a kind of nano-sized carbon mixes aeroge, comprising the following steps:
Under the conditions of anhydrous and oxygen-free, metallic sodium is mixed with the organic solvent containing naphthalene sodium, obtains the electronics of the counter ion containing sodium
Solution；
The electronics solution of part counter ion containing sodium is mixed with carbon nanotube, obtains carbon nanotube polyanion solution；
The electronics solution of residue counter ion containing sodium is mixed with nitrogen carbide, obtains nitrogen carbide polyanion solution；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed and be crosslinked instead
It answers, obtains nano-sized carbon and mix aeroge.
Preferably, the organic solvent is anhydrous dimethylacetamide, dimethylformamide or liquid ammonia.
Preferably, the molar ratio of the sodium ion in the electronics solution of part counter ion containing sodium and carbon nanotube is 1:4
~100.
Preferably, the molar concentration of the sodium ion in the electronics solution of part counter ion containing sodium be 0.01~
0.1mol/L。
Preferably, the molar ratio of the sodium ion in the electronics solution of the remaining counter ion containing sodium and nitrogen carbide be 1:2~
16。
Preferably, the molar concentration of the sodium ion in the electronics solution of the remaining counter ion containing sodium be 0.006~
0.06mol/L。
Preferably, the sum of sodium ion in the carbon nanotube polyanion solution and nitrogen carbide polyanion solution and two
The molar ratio of iodobenzene is 1:1.
Preferably, the time of the cross-linking reaction is 15min~for 24 hours.
The present invention also provides nano-sized carbons made from preparation method described in above-mentioned technical proposal to mix aeroge.
The present invention also provides nano-sized carbons described in above-mentioned technical proposal to mix application of the aeroge in electro-catalysis field.
The present invention provides the preparation methods that a kind of nano-sized carbon mixes aeroge, comprising the following steps: in anhydrous and oxygen-free item
Under part, metallic sodium is mixed with the organic solvent containing naphthalene sodium, obtains the electronics solution of the counter ion containing sodium；By part counter ion containing sodium
Electronics solution mixed with carbon nanotube, obtain carbon nanotube polyanion solution；By the electronics solution of residue counter ion containing sodium
It is mixed with nitrogen carbide, obtains nitrogen carbide polyanion solution；By the carbon nanotube polyanion solution, nitrogen carbide polyanion
Solution and diiodo-benzene mixing carry out cross-linking reaction, obtain nano-sized carbon and mix aeroge.The present invention is by FL-CNs and conductive nanometer
Carbon material (carbon nanotube) mixes, and the ultralight nano-sized carbon for preparing three-dimensional porous high conductivity mixes aeroge, airsetting obtained
Glue can be used as the electrode of high conductivity energy storage device in terms of electrochemical energy storage；It, both can be directly as urging in terms of catalysis characteristics
Agent uses, and can effectively improve catalysis as catalyst carrier by function dough or loading functional nanoparticle and make
With due to high-specific surface area and high nitrogen active site, so that the material high catalytic efficiency, can be effectively reduced the use of noble metal catalyst
Amount；Meanwhile being also used to high-end heat-insulation and heat-preservation system etc..
Detailed description of the invention:
Nano-sized carbon made from Fig. 1 embodiment 1 mixes the characterization spectrogram of aeroge, wherein (a) is SEM spectrogram, it is (b) implementation
Nano-sized carbon made from example 1 mixes SEM spectrogram of the aeroge as catalyst made from catalyst carrier, (c) is nanometer platinum catalysis
The average grain diameter and size distribution plot of agent；
Fig. 2 is that platinum catalyst mixes aeroge carrier in nitrogen carbide, redox graphene and nano-sized carbon and platinum/carbon is urged
The current density plot in the oxygen reduction reaction overvoltage section of agent carrier；
Fig. 3 is the optical photograph that nano-sized carbon made from embodiment 1 mixes aeroge；
Fig. 4 is the high-resolution SEM spectrogram that nano-sized carbon made from embodiment 1 mixes aeroge；
Fig. 5 is gap distribution and the specific surface area curve that nano-sized carbon made from embodiment 1 mixes aeroge；
Fig. 6 is the conductivity and Raman spectrum defect map that nano-sized carbon made from embodiment 1 mixes aeroge；
Fig. 7 is the energy storage characteristic curve that nano-sized carbon made from the present embodiment mixes aeroge for energy storage device.
Specific embodiment
The present invention provides the preparation methods that a kind of nano-sized carbon mixes aeroge, comprising the following steps:
Under the conditions of anhydrous and oxygen-free, metallic sodium is mixed with the organic solvent containing naphthalene sodium, obtains the electronics of the counter ion containing sodium
Solution；
The electronics solution of part counter ion containing sodium is mixed with carbon nanotube, obtains carbon nanotube polyanion solution；
The electronics solution of residue counter ion containing sodium is mixed with nitrogen carbide, obtains nitrogen carbide polyanion solution；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed and be crosslinked instead
It answers, obtains nano-sized carbon and mix aeroge.
The present invention mixes under the conditions of anhydrous and oxygen-free, by metallic sodium with the organic solvent containing naphthalene sodium, obtains counter ion containing sodium
Electronics solution.In the present invention, the organic solvent is preferably anhydrous dimethylacetamide, dimethylformamide or liquid
Ammonia.The electronics solution that the counter ion containing sodium is prepared in the present invention can use spontaneous electrostatic stripping process, form carbon nanotube or carbon
The polyanion electrolyte for changing nitrogen, reduces other chemistry (oxidation removing etc.) or physics removing (ultrasonic disperse etc.) mode receives carbon
The damage of mitron and nitrogen carbide keeps the monodisperse status of material, prevents cross-linking process to its specific surface area and pore morphology shadow
It rings, avoids the reunion again or stacking of having removed carbon nanotube and nitrogen carbide group element material.
The present invention does not have special restriction to the concentration of the naphthalene sodium in the organic solvent containing naphthalene sodium.
After obtaining the electronics solution of the counter ion containing sodium, the present invention is by the electronics solution and carbon nanotube of part counter ion containing sodium
Mixing, obtains carbon nanotube polyanion solution.In the present invention, the sodium in the electronics solution of part counter ion containing sodium from
Son and the molar ratio of carbon nanotube are preferably 1:4~100, more preferably 1:10~12.
In the present invention, the molar concentration of the sodium ion in the electronics solution of part counter ion containing sodium is preferably 0.01
~0.1mol/L, more preferably 0.025~0.043mol/L.Mixed process will drive alkali metal ion sodium ion quickly from charge
Transfer agent-naphthols is transferred to interstitial site, and obtained carbon nanotube polyanion electrolyte spontaneous can be dissolved in organic molten
In agent, by the electrically charged amount of control group element material skeleton (the electronics solution of the counter ion containing sodium) institute, high degree of dispersion, high concentration are formed
Solution.
In the present invention, the concentration of carbon nanotube is preferably 0.5~6.5mg/ in the carbon nanotube polyanion solution
ML, more preferably≤2mg/mL.
In the present invention, the diameter of the carbon nanotube is preferably smaller than 50nm, and the Raman G/D of the carbon nanotube is than preferred
>100.In the present invention, the carbon nanotube is preferably single-walled carbon nanotube.The present invention does not have the source of the carbon nanotube
Special restriction, using commercial goods well known to those skilled in the art.
After obtaining the electronics solution of the counter ion containing sodium, the present invention mixes the electronics solution of residue counter ion containing sodium with nitrogen carbide
It closes, obtains nitrogen carbide polyanion solution.In the present invention, the sodium ion in the electronics solution of the remaining counter ion containing sodium with
The molar ratio of nitrogen carbide is preferably 1:2~16, more preferably 1:5~8, most preferably 1:7.1.
In the present invention, the molar concentration of the sodium ion in the electronics solution of the remaining counter ion containing sodium is preferably
0.006~0.06mol/L, more preferably 0.012~0.020mol/L, most preferably 0.015mol/L.Mixed process will drive
Alkali metal ion sodium ion is quickly transferred to interstitial site, obtained nitrogen carbide polyanion electricity from charge transfer agent-naphthols
Solution matter spontaneous can be dissolved in organic solvent, be charged by controlling group element material skeleton (the electronics solution of the counter ion containing sodium)
Lotus amount forms the solution of high degree of dispersion, high concentration.
In the present invention, the concentration of nitrogen carbide is preferably 0.5~4mg/mL in the nitrogen carbide polyanion solution, more excellent
It is selected as≤3.5mg/mL.
In the present invention, the nitrogen carbide is preferably the lamellar structure nitrogen carbide of highly crystalline, in the carbonitride nitrogen with
Carbon atomic ratio is preferred > and 1.In the present invention, the diameter of the nitrogen carbide is preferably 50~100 nanometers.The present invention is to the carbonization
The source of nitrogen does not have special restriction, using commercial goods well known to those skilled in the art.
After obtaining the carbon nanotube polyanion solution and nitrogen carbide polyanion solution, the present invention is by the carbon nanometer
Pipe polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene mixing carry out cross-linking reaction, obtain nano-sized carbon and mix airsetting
Glue.
In the present invention, the sum of the sodium ion in the carbon nanotube polyanion solution and nitrogen carbide polyanion solution
Molar ratio with diiodo-benzene is preferably 1:1.
In the present invention, the time of the cross-linking reaction is preferably 15min~for 24 hours, and the temperature of the cross-linking reaction is preferred
For room temperature, additional heating or cooling are not needed.
The present invention also provides nano-sized carbons made from preparation method described in above-mentioned technical proposal to mix aeroge.In the present invention
In, the nano-sized carbon, which mixes aeroge, which to be led, has that electric rate is high, specific surface area height and the big advantage of size.
The present invention also provides nano-sized carbons described in above-mentioned technical proposal to mix application of the aeroge in electro-catalysis field.?
In the present invention, the application is preferably included: in terms of electrochemical energy storage, the electrode as high conductivity energy storage device；It is being catalyzed
In terms of characteristic, it can not only be used directly as catalyst, but also can be by function dough or loading functional nanoparticle, as catalysis
Agent carrier effectively improves catalytic action, due to high-specific surface area and high nitrogen active site, so that the material high catalytic efficiency, can have
Effect reduces the dosage of noble metal catalyst；Meanwhile being also used to high-end heat-insulation and heat-preservation system.
Mix aeroge and its preparation method and application to nano-sized carbon provided by the invention below with reference to embodiment to carry out in detail
Thin explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Under the conditions of anhydrous and oxygen-free, metallic sodium 0.02g is mixed with the anhydrous dimethylacetamide solution 20mL containing naphthalene sodium,
The electronics solution of the counter ion containing sodium is obtained, the mass concentration of naphthols is 6.6mg/ in the anhydrous dimethylacetamide solution containing naphthalene sodium
mL；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 5mL and carbon nanotube of part counter ion containing sodium
0.026g (single-walled carbon nanotube, the diameter of carbon nanotube are 0.8~1.3nm, ratio > 100 Raman G/D) mixing, obtains carbon nanometer
Pipe polyanion solution；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 7mL of residue counter ion containing sodium and nitrogen carbide 0.028g
(lamellar structure nitrogen carbide, nitrogen and carbon atomic ratio > 1, diameter are 50 nanometers) mixing, obtains nitrogen carbide polyanion solution；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed in room temperature and handed over
Connection reaction for 24 hours, obtains nano-sized carbon and mixes aeroge, the sodium in carbon nanotube polyanion solution and nitrogen carbide polyanion solution
The molar ratio of the sum of ion and diiodo-benzene is 1:1.
Aeroge is mixed to nano-sized carbon made from the present embodiment and carries out sem analysis, as a result as shown in Fig. 1 (a), this is implemented
Nano-sized carbon made from example mixes aeroge and catalyst is made for the catalyst carrier in direct methanol fuel cell, to catalyst
Sem analysis is carried out, as a result as shown in Fig. 1 (b), Fig. 1 (c) is the average grain diameter and size distribution plot of nm Pt catalyst, by Fig. 1
It is found that noble metal catalyst is more uniformly spread.
Fig. 2 is that the hydrogen reduction that platinum catalyst mixes aeroge carrier in nitrogen carbide, redox graphene and nano-sized carbon is anti-
Answer overvoltage section and its business with platinum/carbon catalyst support performance (current density) compare, as seen from Figure 2, this
Nano-sized carbon made from inventing, which mixes aeroge, can greatly improve current density and electro catalytic activity, reduce noble metal catalyst and use
Amount.
Fig. 3 is the optical photograph that nano-sized carbon made from the present embodiment mixes aeroge；Fig. 4 is nanometer made from the present embodiment
Carbon mixes the high-resolution SEM spectrogram of aeroge, and as shown in Figure 4, it is equal that nano-sized carbon mixes carbon nanotube and nitrogen carbide in aeroge
Even distribution, crosslinking become overall structure.
Fig. 5 is gap distribution and the specific surface area curve that nano-sized carbon made from the present embodiment mixes aeroge, can by Fig. 5
Know, which mixes aeroge and sufficiently maintain the big feature of nano-carbon material surface area, specific surface area height and therebetween hole
Gap is nanoscale.
Fig. 6 is the conductivity and Raman spectrum defect analysis that nano-sized carbon made from the present embodiment mixes aeroge, can by Fig. 6
Know, nano-sized carbon made from the present embodiment mixes that aeroge is highly conductive, and defect is few.
Fig. 7 is that nano-sized carbon made from the present embodiment mixes aeroge for energy storage device, the energy storage characteristic curve measured, by
For Fig. 7 it is found that nano-sized carbon made from the present embodiment mixes aeroge as energy-storage capacitor electrode material, TBAP/ acetonitrile is organic
Specific capacitance characteristic may be up to 333F/g in electrolyte.
Embodiment 2
Under the conditions of anhydrous and oxygen-free, metallic sodium 0.06g is mixed with the anhydrous dimethylacetamide solution containing naphthalene sodium, is obtained
The electronics solution of the counter ion containing sodium, the mass concentration of naphthols is 6.6mg/mL in the anhydrous dimethylacetamide solution containing naphthalene sodium；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 23mL and carbon nanotube of part counter ion containing sodium
0.048g (single-walled carbon nanotube, the diameter of carbon nanotube are 0.8`1.3nm, ratio > 100 Raman G/D) mixing, obtains carbon nanotube
Polyanion solution；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 23mL and nitrogen carbide of residue counter ion containing sodium
0.066g (lamellar structure nitrogen carbide, nitrogen and carbon atomic ratio > 1, diameter are 50 nanometers) mixing, it is molten to obtain nitrogen carbide polyanion
Liquid；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed in room temperature and handed over
Connection reaction 15min, obtains nano-sized carbon and mixes aeroge, in carbon nanotube polyanion solution and nitrogen carbide polyanion solution
The molar ratio of the sum of sodium ion and diiodo-benzene is 1:1.
Embodiment 3
Under the conditions of anhydrous and oxygen-free, metallic sodium 0.02g is mixed with the anhydrous dimethylacetamide solution containing naphthalene sodium, is obtained
The electronics solution of the counter ion containing sodium, the mass concentration of naphthols is 6.6mg/mL in the anhydrous dimethylacetamide solution containing naphthalene sodium；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 4mL of part counter ion containing sodium and carbon nanotube 0.2g
(single-walled carbon nanotube, the diameter of carbon nanotube are 0.8~1.3nm, ratio > 100 Raman G/D) mixing, obtains the poly- yin of carbon nanotube
Solion；
By electronics solution (the concentration 0.043mmol/mL of the sodium ion) 4mL of residue counter ion containing sodium and nitrogen carbide 0.018g
(lamellar structure nitrogen carbide, nitrogen and carbon atomic ratio > 1, diameter are 50 nanometers) mixing, obtains nitrogen carbide polyanion solution；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed in room temperature and handed over
Connection reaction 15min, obtains nano-sized carbon and mixes aeroge, in carbon nanotube polyanion solution and nitrogen carbide polyanion solution
The molar ratio of the sum of sodium ion and diiodo-benzene is 1:1.
The aerogel products that embodiment produces have insulation characteristic.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. the preparation method that a kind of nano-sized carbon mixes aeroge, which comprises the following steps:
Under the conditions of anhydrous and oxygen-free, metallic sodium is mixed with the organic solvent containing naphthalene sodium, obtains the electronics solution of the counter ion containing sodium；
The electronics solution of part counter ion containing sodium is mixed with carbon nanotube, obtains carbon nanotube polyanion solution；
The electronics solution of residue counter ion containing sodium is mixed with nitrogen carbide, obtains nitrogen carbide polyanion solution；
The carbon nanotube polyanion solution, nitrogen carbide polyanion solution and diiodo-benzene are mixed and carry out cross-linking reaction, is obtained
Mix aeroge to nano-sized carbon.
2. preparation method described in claim 1, which is characterized in that the organic solvent is anhydrous dimethylacetamide, diformazan
Base formamide or liquid ammonia.
3. preparation method according to claim 1, which is characterized in that in the electronics solution of part counter ion containing sodium
The molar ratio of sodium ion and carbon nanotube is 1:4~100.
4. preparation method according to claim 1 or 3, which is characterized in that the electronics solution of part counter ion containing sodium
In sodium ion molar concentration be 0.01~0.1mol/L.
5. preparation method according to claim 1, which is characterized in that in the electronics solution of residue counter ion containing sodium
The molar ratio of sodium ion and nitrogen carbide is 1:2~16.
6. preparation method according to claim 1 or 5, which is characterized in that the electronics solution of residue counter ion containing sodium
In sodium ion molar concentration be 0.006~0.06mol/L.
7. preparation method according to claim 1, which is characterized in that the carbon nanotube polyanion solution and nitrogen carbide
The molar ratio of the sum of sodium ion in polyanion solution and diiodo-benzene is 1:1.
8. preparation method according to claim 1, which is characterized in that the time of the cross-linking reaction is 15min~for 24 hours.
9. nano-sized carbon made from preparation method described in claim 1~8 any one mixes aeroge.
10. nano-sized carbon as claimed in claim 9 mixes application of the aeroge in electro-catalysis field.
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