CN107651687A - A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen - Google Patents
A kind of preparation method and applications of the Carbon Materials rich in pyridine nitrogen Download PDFInfo
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- CN107651687A CN107651687A CN201711138827.9A CN201711138827A CN107651687A CN 107651687 A CN107651687 A CN 107651687A CN 201711138827 A CN201711138827 A CN 201711138827A CN 107651687 A CN107651687 A CN 107651687A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention provides a kind of preparation method of the Carbon Materials rich in pyridine nitrogen, including synthesis step and activation step；Synthesis step is：Using water plant Enteromorpha as carbon source, mixed solution that carbon source and solvent are formed carries out high pressure hydro-thermal carbon compound into obtaining carbide；Activation step is：Carbide, melamine and potassium hydroxide are heated up in a nitrogen atmosphere according to a certain ratio, is washed after cooling and is drying to obtain the Carbon Materials rich in pyridine nitrogen.The Carbon Materials obtained using the inventive method, effect are：Carbon source abundance is renewable, and itself just contains pore structure and nitrogen, beneficial to the Carbon Materials rich in pyridine nitrogen；Preparation process is simple, and technological parameter is easily controlled, beneficial to industrial applications；Carbon Materials have high nitrogen element content, micron pore size and high-specific surface area feature.Invention additionally discloses a kind of application of above-mentioned Carbon Materials, has in carbon dioxide adsorption, electrocatalytic reaction and electrode material production field and is widely applied very much prospect.
Description
Technical field
The present invention relates to field of material technology, especially, is related to a kind of preparation side of the Carbon Materials rich in pyridine nitrogen
Method and its application.
Background technology
Porous carbon material is due to its higher specific surface area and flourishing pore passage structure, good electric conductivity, resistance to acids and bases
It is strong and stable in certain temperature range inner structure and be widely used in separation/purifying of material, catalyst carrier, electrode material
The fields such as material, medical carrier.
At present, preparing the method for porous carbon material both at home and abroad mainly includes traditional carbonization-activation method and template：
1st, the obtained often unordered porous carbon material of activation method, it is difficult to control its duct shape and aperture.
2nd, template must first synthesize the soft template (high molecular polymer) or hard template metal organic framework as template
(MOF) etc..
Above two method, which prepares Carbon Materials, has following defect：(1) raw material is not easy to obtain, expensive；(2) aperture point
Cloth is poor (some apertures are bigger than normal)；(3) complex steps, the difficult control of technological parameter；(4) surface area is relatively low, and some surfaces are unsupported
Hetero atom causes its electric conductivity and wetability poor.In addition, the nitrogen-doping porous carbon material being prepared is studied at present very
It is rare report pyridine nitrogen element structure, and pyridine nitrogen to chemical property have greatly facilitate effect.Therefore, prior art makes
It is poor as supercapacitor applications chemical property to obtain it, or it is not high as sorbing material absorption property, or in actual industrial
In be difficult to largely produce.
Therefore, design that a kind of manufacture craft is simplified, technological parameter is easily controlled and can in high volume obtain rich in pyridine nitrogen member
The preparation method of the Carbon Materials of element is significant.
The content of the invention
The first object of the present invention is to provide that a kind of manufacture craft is simplified, technological parameter is easily controlled and can in high volume be obtained
The preparation method of the Carbon Materials of pyridine nitrogen must be rich in, concrete technical scheme is：
A kind of preparation method of the Carbon Materials rich in pyridine nitrogen, including synthesis step and activation step；
The synthesis step is specifically：Using water plant Enteromorpha as carbon source, the mixed solution that carbon source and solvent are formed is put
1-30 hours are incubated under the conditions of 100 DEG C -200 DEG C are warming up in the ptfe autoclave of sealing, as caused by its own
Pressure carries out high pressure solvent thermal synthesis, obtains carbide；
The activation step is specifically：By carbide, melamine and potassium hydroxide according to 1：0.3-2.0：0.5-2.0
Quality proportioning grinding after be placed in crucible, be incubated 2-3h under the conditions of being warming up to 500 DEG C -900 DEG C in a nitrogen atmosphere, heating speed
Rate is 1-10 DEG C/min, is washed after cooling and is drying to obtain the Carbon Materials rich in pyridine nitrogen.
Preferable in above technical scheme, the solvent is at least one in water, ethanol, acetone and dilution heat of sulfuric acid
Kind, the mass fraction of sulfuric acid is 1%-5% in dilution heat of sulfuric acid；180 DEG C are warming up in the synthesis step, is incubated 24h.
It is preferable in above technical scheme, in the activation step：The quality of carbide, melamine and potassium hydroxide
Match as 1：1：2.0；2h is incubated under the conditions of being warming up to 800 DEG C, heating rate is 2 DEG C/min.
It is preferable in above technical scheme, in the Carbon Materials rich in pyridine nitrogen：Nitrogen element content is 1.4-
15.6at%, aperture 0.5-3.0nm, specific surface area 900-2000m2/g。
In above technical scheme preferably, in addition to pre- carburising step, the pre- carburising step are specifically：By the synthesis
Carbide obtained by step is warming up to 300 DEG C -600 DEG C under nitrogen atmosphere, is incubated 1-3h, heating rate is 1-10 DEG C/min.
It is preferable in above technical scheme, in the pre- carburising step：450 DEG C are warming up to, is incubated 1h, heating rate 4
℃/min。
In above technical scheme preferably, in addition to feed pretreatment step, the feed pretreatment step are specifically：Will
The biomass raw material collected carry out washing and freeze-drying process obtains carbon source.
Preferable in above technical scheme, the detailed process of the washing and drying process is：A, by the Enteromorpha (water of collection
Plant Enteromorpha) first handled 2 hours at 60 DEG C with 2mol/L hydrochloric acid solution；B, the Enteromorpha after processing is washed with deionized
To neutrality；C, the Enteromorpha after washing is directly immersed in liquid nitrogen environment and carries out quick freeze；D, the Enteromorpha after freezing is placed in freezing
Freeze-drying process 3 days in drying machine, obtain dry carbon source.
Using the preparation method of the present invention, effect is：
1st, for the present invention using water plant Enteromorpha as carbon source, the carbon source abundance is renewable, and itself is just tied containing hole
Structure and nitrogen (difference for having essence with the raw material such as disclosed stalk, root of kudzu vine in the prior art), beneficial to rich in pyridine nitrogen
Carbon Materials.
2nd, preparation method of the invention includes synthesis step and activation step, realizes that a step activation method obtains being rich in pyridine nitrogen
The Carbon Materials of element, preparation process is relatively easy, and technological parameter is easily controlled, beneficial to industrial applications.
3rd, in the Carbon Materials rich in pyridine nitrogen obtained by the present invention：Nitrogen element content is 1.4-15.6at%, hole
Footpath is 0.5-3.0nm, specific surface area 900-2000m2/ g so that it is in carbon dioxide adsorption, making capacitor electrode material
And electrocatalytic oxidation reduction reaction field have be widely applied very much prospect.
4th, present invention additionally comprises feed pretreatment step, the raw material that the method handles to obtain remains in that Enteromorpha green in itself
Color and fluffy shape (particularly Freeze Drying Technique can be good at keeping the pore passage structure in raw material inherently), and adopt
Substantially grayed with the sunshine irradiation raw material color that either baking oven high temperature drying obtains, and the duct of raw material inherently
Structure is substantially destroyed.
The invention also discloses a kind of application of the above-mentioned Carbon Materials rich in pyridine nitrogen, specifically available for titanium dioxide
At least one of in carbon adsorption, making capacitor electrode material and electrocatalytic oxidation reduction reaction, it is practical.
In addition to objects, features and advantages described above, the present invention also has other objects, features and advantages.
Below with reference to accompanying drawings, the present invention is further detailed explanation.
Brief description of the drawings
The accompanying drawing for forming the part of the application is used for providing a further understanding of the present invention, schematic reality of the invention
Apply example and its illustrate to be used to explain the present invention, do not form inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is the pore size distribution curve figure of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 2 (a) is the XPS spectrum figure of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 2 (b) is the N1s spectrograms of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 3 (a) is the SEM figures of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 3 (b) is the TEM figures of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 3 (c) is Fig. 3 (b) partial enlarged drawing；
Fig. 4 is the isothermal adsorption heating curve of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 5 (a) is the cyclic voltammetry curve under the Carbon Materials different scanning rates rich in pyridine nitrogen in embodiment 1
Figure；
Fig. 5 (b) is the charging and discharging curve figure of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 6 (a) is circulation of the Carbon Materials rich in pyridine nitrogen in nitrogen and oxygen saturation electrolyte in embodiment 1
Volt-ampere curve figure；
Fig. 6 (b) is the linear scan curve map under the Carbon Materials different rotating speeds rich in pyridine nitrogen in embodiment 1；
Fig. 7 (a) is that the Carbon Materials rich in pyridine nitrogen are the methanol tolerance performance map after addition methanol in embodiment 1；
Fig. 7 (b) is the attenuation curve figure of the Carbon Materials rich in pyridine nitrogen in embodiment 1；
Fig. 8 is the nitrogen adsorption isotherm of sample and pore size distribution curve figure in comparative example 1；
Fig. 9 is sample CO at 0 and 25 DEG C in comparative example 12Adsorption isotherm and isothermal adsorption heating curve figure；
Figure 10 is the N element XPS swarming curve maps of sample in comparative example 1.
Embodiment
Embodiments of the invention are described in detail below in conjunction with accompanying drawing, but the present invention can limit according to claim
Fixed and covering multitude of different ways is implemented.
Embodiment 1：
A kind of preparation method of the Carbon Materials rich in pyridine nitrogen, it is specifically：
The first step, feed pretreatment step, it is specifically：The biomass raw material Enteromorpha collected is subjected to pickling, water
Wash and freeze-drying process, detailed process are：A, it is the Enteromorpha of collection is first small in 60 DEG C of processing 2 with 2mol/L hydrochloric acid solution
When；B, the Enteromorpha after processing is washed with deionized to neutrality；C, the Enteromorpha after washing is directly immersed in into liquid nitrogen environment to carry out
Quick freeze；D, the Enteromorpha after freezing is placed in freeze-drying process 3 days in freeze drier, obtains dry carbon source；
Second step, synthesis step, it is specifically：Taking appropriate carbon source, (preferably polytetrafluoroethylene is anti-in 100mL hydrothermal reaction kettles
Answer kettle, typically use 1L solvent burden ratio 10-80g carbon sources) in, add deionized water to reactor 2/3 (the three of volume/
Two)；It is warming up to 180 DEG C；High pressure hydro-thermal carbon compound is carried out into reaction 24h by its own caused pressure, obtains carbide；
3rd step, pre- carburising step, it is specifically：Nitrogen will be placed directly within after carbide washing and 120 DEG C of dryings of a conventional oven
450 DEG C are warming up under gas atmosphere, is incubated 2h, heating rate is 4 DEG C/min, further obtains pre- carbide；
4th step, activation step, it is specifically：By pre- carbide, melamine and potassium hydroxide using mass ratio as 1：1：2
It is placed in after ratio grinding in crucible, is warming up to 800 DEG C in a nitrogen atmosphere, keeps 2h, heating rate is 2 DEG C/min, obtains richness
The Carbon Materials of the nitrogen containing pyridine, labeled as ANC-800.
Detected or tested using the Carbon Materials (ANC-800) rich in pyridine nitrogen obtained by the present embodiment, details are such as
Under：
1st, the pore-size distribution of Carbon Materials (ANC-800) refers to Fig. 1, and as shown in Figure 1, the Carbon Materials obtained by the present embodiment are micro-
Hole, and pore-size distribution, than more uniform, main peak is located at 2.5nm or so.
2nd, XPS (x-ray photoelectron power spectrum) spectrogram of Carbon Materials (ANC-800) refers to Fig. 2 (a) obtained by the present embodiment, its
N1s spectrograms refer to Fig. 2 (b).It can clearly be seen that containing carbon, nitrogen, the element of oxygen three, i.e. nitrogen is successfully doped to from Fig. 2 (a)
In porous carbon material.From Fig. 2 (b) it can be seen that nitrogen is mainly made up of pyridine nitrogen, pyrroles's nitrogen and graphitization N structure, especially
It is the pyridine nitrogen content highest positioned at 398.3eV.
3rd, the SEM figures of Carbon Materials (ANC-800) refer to Fig. 3 (a) obtained by the present embodiment, its TEM figures, refer to Fig. 3 (b) and figure
3 (c) (wherein Fig. 3 (c) is Fig. 3 (b) partial enlarged drawing), it can be seen that this kind of Carbon Materials have spherical shape shape from Fig. 3 (a)
Looks, it was demonstrated that it is charcoal ball that it is carbohydrate-modifying, which can to effectively facilitate the cellulose itself contained etc., for hydro-thermal process, and this is also first
Reported in the secondary Carbon Materials obtained in biomass material, charcoal is typically readily obtained as carbon source using carbohydrate such as glucose
Ball.It can be seen that this kind of Carbon Materials have equally distributed pore size in Fig. 3 (b) and Fig. 3 (c).
4th, the absorption figure of Carbon Materials (ANC-800) progress carbon dioxide adsorption obtained by the present embodiment refers to Fig. 4 and (inhaled for isothermal
Attached heating curve), figure 4, it is seen that the Carbon Materials (ANC-800) of the present embodiment are good to the absorption property of carbon dioxide, tool
Body is：CO under normal temperature and pressure2Adsorbance is up to 3.0mmol/g, and especially thermostatic absorption heat is up to 40kJ/mol, it was demonstrated that micropore
Size and alkaline nitrogen and CO2Intermolecular active force is stronger.
5th, Carbon Materials (ANC-800) obtained by the present embodiment are assembled into ultracapacitor, its performance refers to Fig. 5 (a) and Fig. 5
(b), Fig. 5 (a) is the cyclic voltammetry curve under different scanning rates, and Fig. 5 (b) is charging and discharging curve, it is known that：The charcoal of the present embodiment
It is good that material (ANC-800) is assembled into performance of the supercapacitor, especially good cycling stability, is still protected after circulation 10000 times
Hold up to 98% current efficiency.
6th, Carbon Materials (ANC-800) are applied in 0.1mol/L potassium hydroxide electrolyte obtained by the present embodiment, its performance
Fig. 6 (a) and Fig. 6 (b) are referred to, Fig. 6 (a) is the cyclic voltammetry curve of electrolyte under nitrogen and oxygen-saturated conditions, it was demonstrated that is had
Hydrogen reduction catalytic performance；Fig. 6 (b) is the linear scan curve under different rotating speeds, it can be seen that current density is with sweep speed
Increase and increase, it was demonstrated that this Carbon Materials belong to anti-with good diffusion effect, particularly hydrogen reduction to oxygen reduction reaction
Electron transfer number during answering is 3.79, and close to 4, therefore hydrogen reduction process is converted mainly into H2O, only produce on a small quantity
H2O2。
7th, the electro-catalysis curve of Carbon Materials (ANC-800) obtained by the present embodiment and commercialization Pt/C electrodes refer to Fig. 7 (a) and
Fig. 7 (b), Fig. 7 (a) are the methanol tolerance performance after addition methanol, it was demonstrated that its methanol tolerance function admirable, methanol are anti-to electrode oxygen reduction
It should have little to no effect, and be commercialized platinum carbon resistance rod as the addition of methanol shows obvious Section Effect；Fig. 7 (b) is to decline
Subtract curve, it was demonstrated that 91.1% performance is remained in that after reaction 20000s, better than commercialization platinum carbon resistance rod.
8th, understood with reference to comparative example and the embodiment of the present invention 1, the present invention uses the group of potassium hydroxide and melamine
Close and realize that the activation process of pre- carbide has substantial influence to the final Carbon Materials for being rich in pyridine nitrogen that can obtain, and
Significant effect.
Embodiment 2
Difference from Example 1 is：600 DEG C are warming up in activation step, that is, obtains the charcoal rich in pyridine nitrogen
Material, labeled as ANC-600, its performance is compared with ANC-800：Nitrogen content is higher, but BET specific surface area is relatively low, causes it
CO2Adsorbance is relatively low, and capacitance is relatively low.
Embodiment 3
Difference from Example 1 is：700 DEG C are warming up in activation step, that is, obtains the charcoal rich in pyridine nitrogen
Material, labeled as ANC-700, its performance is compared with ANC-800：Nitrogen content is higher, but BET specific surface area is relatively low, causes it
CO2Adsorbance is relatively low, and capacitance is relatively low.
Comparative example
The present embodiment difference from Example 1 is：Melamine is not added with activation step, will pre- carbide
With potassium hydroxide using mass ratio as 1：2 ratio carries out being mixed to get activator mixture.
, with embodiment 1, obtained Carbon Materials are designated as AHC-800 for other.
The Carbon Materials effect obtained according to comparative example method is：
(1) nitrogen adsorption isotherm of AHC-800 samples and pore size distribution curve refer to Fig. 8, as can be seen from Figure 8：Hole
Footpath Size Distribution is wider, not single micropore distribution.
(2) AHC-800 samples CO at 0 and 25 DEG C2Adsorption isotherm and isothermal adsorption heating curve figure refer to Fig. 9, can be with
It was found that because specific surface area is larger, although adsorbance is higher than NAC-800, its heat of adsorption is only 32kJ/mol, mainly because
It is relatively low wider caused with pore-size distribution for nitrogen element content.
(3) nitrogen XPS swarming curve maps refer to Figure 10 in AHC-800 samples, as can be seen from the figure：Carbon Materials nitrogen member
Cellulose content is relatively low；It can be seen that nitrogen is mainly made up of pyridine nitrogen, pyrroles's nitrogen and graphitization N structure, especially it is located at
403.1eV pyrroles's nitrogen content highest, with notable difference compared with embodiment 1.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (9)
- A kind of 1. preparation method of the Carbon Materials rich in pyridine nitrogen, it is characterised in that：Including synthesis step and activation step；The synthesis step is specifically：Using water plant Enteromorpha as carbon source, the mixed solution that carbon source and solvent are formed is placed in close 1-30 hours are incubated under the conditions of 100 DEG C -200 DEG C are warming up in the ptfe autoclave of envelope, by its own caused pressure High pressure solvent thermal synthesis is carried out, obtains carbide；The activation step is specifically：By carbide, melamine and potassium hydroxide according to 1：0.3-2.0：0.5-2.0 matter It is placed in after amount proportioning grinding in crucible, 2-3h is incubated under the conditions of being warming up to 500 DEG C -900 DEG C in a nitrogen atmosphere, heating rate is 1-10 DEG C/min, washed after cooling and be drying to obtain the Carbon Materials rich in pyridine nitrogen.
- 2. the preparation method of the Carbon Materials according to claim 1 rich in pyridine nitrogen, it is characterised in that：The solvent For at least one of water, ethanol, acetone and dilution heat of sulfuric acid, the mass fraction of sulfuric acid is 1%-5% in dilution heat of sulfuric acid； 180 DEG C are warming up in the synthesis step, is incubated 24h.
- 3. the preparation method of the Carbon Materials according to claim 2 rich in pyridine nitrogen, it is characterised in that：The activation In step：The quality proportioning of carbide, melamine and potassium hydroxide is 1：1：2.0；It is incubated under the conditions of being warming up to 800 DEG C 2h, heating rate are 2 DEG C/min.
- 4. the preparation method of the Carbon Materials according to claim 1 rich in pyridine nitrogen, it is characterised in that：It is described to be rich in Nitrogen element content is 1.4-15.6at% in the Carbon Materials of pyridine nitrogen, aperture size 0.5-3.0nm, and specific surface area is 900-2000m2/g。
- 5. the preparation method of the Carbon Materials rich in pyridine nitrogen according to claim 1-4 any one, its feature exist In：Also include pre- carburising step, the pre- carburising step is specifically：By the carbide obtained by the synthesis step in nitrogen atmosphere Under be warming up to 300 DEG C -600 DEG C, be incubated 1-3h, heating rate is 1-10 DEG C/min.
- 6. the preparation method of the Carbon Materials according to claim 5 rich in pyridine nitrogen, it is characterised in that：The pre- carbon Change in step：450 DEG C are warming up to, is incubated 1h, heating rate is 4 DEG C/min.
- 7. the preparation method of the Carbon Materials according to claim 5 rich in pyridine nitrogen, it is characterised in that：Also include original Expect pre-treatment step, the feed pretreatment step is specifically：The biomass raw material collected are washed and freezed Drying process obtains carbon source.
- 8. the preparation method of the Carbon Materials according to claim 7 rich in pyridine nitrogen, it is characterised in that：The washing Detailed process with drying process is：A, the Enteromorpha of collection is first handled 2 hours with 2mol/L hydrochloric acid solution at 60 DEG C；B, will Enteromorpha after processing is washed with deionized to neutrality；C, by the Enteromorpha after washing be directly immersed in liquid nitrogen environment carry out it is rapid cold Freeze；D, the Enteromorpha after freezing is placed in freeze-drying process 3 days in freeze drier, obtains dry carbon source.
- A kind of 9. application of the Carbon Materials rich in pyridine nitrogen as described in claim 1-8 any one, it is characterised in that：With At least one of in carbon dioxide adsorption, making capacitor electrode material and electrocatalytic oxidation reduction reaction.
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| CN110449129A (en) * | 2019-07-22 | 2019-11-15 | 长江大学 | A kind of method and its application of soapberry residue preparation hydro-thermal charcoal |
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| CN111017927A (en) * | 2020-01-08 | 2020-04-17 | 浙江大学 | Preparation and application method of nitrogen-doped porous carbon based on straw hydrothermal carbonization |
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| CN109499599A (en) * | 2018-12-11 | 2019-03-22 | 中国科学院理化技术研究所 | A kind of pyridine nitrogen enrichment carbon nano-tube catalyst and its preparation method and application |
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| CN110449129A (en) * | 2019-07-22 | 2019-11-15 | 长江大学 | A kind of method and its application of soapberry residue preparation hydro-thermal charcoal |
| CN110860274A (en) * | 2019-11-19 | 2020-03-06 | 南京工程学院 | Method for preparing adsorption coke by using waste lile pillow |
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Application publication date: 20180202 |