CN109665525A - A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon - Google Patents
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon Download PDFInfo
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- CN109665525A CN109665525A CN201910091549.9A CN201910091549A CN109665525A CN 109665525 A CN109665525 A CN 109665525A CN 201910091549 A CN201910091549 A CN 201910091549A CN 109665525 A CN109665525 A CN 109665525A
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- iron nitrogen
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
Abstract
The present invention provides a kind of preparation methods of " dumbbell shape " iron nitrogen codope porous carbon, including prepare hydro-thermal carbon sample by raw material of carbon source, iron nitrogen dopant and surfactant；It is handled in protective gas atmosphere through high temperature cabonization later and chemical activation is handled, obtain " dumbbell shape " iron nitrogen codope porous carbon.The advantages that conductive height of " dumbbell shape " iron nitrogen codope porous carbon prepared by the present invention, specific surface area and pore volume are adjustable, and iron nitrogen content is controllable, is conducive to the optimization that its physical and chemical performance is realized by the regulation to its structure." dumbbell shape " iron nitrogen codope porous carbon produced by the present invention has potential application value in fields such as electrode material, separation, absorption, sensing, catalyst carrier and gas storages, the fast development for China's Novel Carbon Nanomaterials that can make greater efforts to promote.
Description
Technical field
The present invention relates to carbon material preparation fields, and in particular to a kind of preparation side of " dumbbell shape " iron nitrogen codope porous carbon
Method.
Background technique
Porous carbon materials are due to low in cost, large specific surface area, pore structure prosperity, acid and alkali-resistance, corrosion-resistant, stability
Properties and the features such as good, excellent conductivity and aperture are adjustable, in terms of the separation, absorption and photoelectricity of macromolecular
It has a wide range of applications.In addition to aforementioned properties, porous carbon materials supercapacitor, lithium ion battery, lithium-sulfur cell and
The fields such as fuel cell also show that tempting prospect.
Currently, the method for synthesis porous carbon materials mainly has hard template method, construction from part and hydro-thermal method etc..Hard template method is usual
Hard template (such as silica, magnesia) is coated using carbon source, the method for removing hard template after carbonization again prepares porous carbon materials,
But this method complex procedures, higher cost, fabrication cycle are long, it is difficult to large-scale production, and using hard template method to preceding
The requirement for driving body and template is relatively high.Construction from part prepare porous carbon materials be it is a kind of synthesized by soluble pore creating material guiding it is porous
The method of carbon material.This method eliminates the step of preparation hard template, and more economical rationality is environmentally protective.This kind of side at present
The resin that method is mainly formed using phenol, formaldehyde by catalysis reaction obtains porous carbon materials by subsequent heat treatment as presoma.
It is most of at present to use monocycle phenol and its synthetic resin as pore former, there is very big limitation to the properties of institute's prepared material,
The property of gained carbon material is also difficult to meet application demand.Hydro-thermal method refers under high-temperature and high-pressure conditions, in a sealed container plus
Entering water makes reactant wherein carry out method of the chemical reaction to obtain carbon material.Compared to traditional preparation methods, hydro-thermal method was both
It is environmentally protective and mild quick, while the preparation process of this method embodies that chemical preparation material is environmentally protective, sustainable development
The thought of exhibition.
Studies have shown that the performance of carbon material various aspects can further be promoted by carrying out activation and doping vario-property to carbon material.Carbon
The method of material activation is broadly divided into two major classes: physical activation method and chemical activation method.Physically activated is to utilize air, titanium dioxide
The oxidizing gas such as carbon, vapor are reacted with carbon atom in carbon material at high temperature；Chemical activation be by chemical reagent such as
ZnCl2、KOH、H3PO4And NH4NO3A series of crosslinking or polycondensation reaction occurs Deng with carbon material, and then creates hole abundant
Gap.Steam activation fast speed, but hardly result in high-specific surface area activated carbon；It is available using carbon dioxide activation
High-specific surface area activated carbon, but its activation temperature is high, speed is slow, therefore energy consumption is very high, and activation time usually requires tens hours,
Even hours up to a hundred.Chemical activation advantage is that activation time is short, activation temperature is low, is conducive to obtain the higher carbon materials of specific surface area
Material；Especially ammonium salt (such as NH4NO3Deng) be used as activator when, can all decompose, not need to clean, carbon material can be effectively controlled
Pore size can also reduce reaction temperature, save electric energy, improve safety.Using miscellaneous element (such as N, P, S, B, Fe) to carbon
Skeleton is doped, and is remarkably improved the surface nature of carbon material, is such as improved wetability, is improved electric conductivity and electrocatalysis characteristic
Deng, be also used as in electrochemistry reaction active site.Moreover, being adulterated relative to single element, multi-element doping in recent years
Significant advantage is had more promoting porous carbon materials aspect of performance.
In addition, the most significant problems faced in porous carbon materials field are how to meet large-scale industrialization demand, separately
On the one hand it is used as a kind of new material, it plays an important role in catalytic field, plays to industrial realization green production important
It influences.
Summary of the invention
The invention proposes a kind of preparation methods of " dumbbell shape " iron nitrogen codope porous carbon, and method is simple, low in cost,
It can be realized industrialized production.
Realize the technical scheme is that
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, steps are as follows:
(1) by carbon source, iron nitrogen dopant and surfactant deionized water dissolving, ultrasonic cleaning is put into after stir process
Ultrasound is carried out in device, hydrothermal reaction kettle is transferred to and carries out hydro-thermal reaction, is cooled to room temperature rear resulting material deionized water filtering and is washed
It washs to neutrality, is put into drying in oven, obtain hydro-thermal carbon sample；
(2) hydro-thermal carbon sample in step (1) is put into tube furnace, in protective gas atmosphere high temperature carbonization treatment, obtains iron
Nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with activator, isometric alcohol and water-soluble is added
Xie Hou is put into baking oven and is dried, and then calcines desciccate in nitrogen gas atmosphere, and deionized water is used in taking-up
It cleans, obtains " dumbbell shape " iron nitrogen codope porous carbon after dry in baking oven.
Carbon source is glucose, sucrose, glycogen or cellulose in the step (1), and iron nitrogen dopant is that six hydrated sulfuric acids are sub-
Iron ammonium, surfactant are neopelex or dodecyl sodium sulfate；Carbon source, iron nitrogen dopant and surfactant
Mass ratio be (20-30): (1-3): 1.
Mixing time is 10-30min, stirring rate 100-200r/min, ultrasonic time 1- in the step (1)
3h, ultrasonic power 100-300W；Hydrothermal temperature is 160-190 DEG C, and the hydro-thermal time is 10-15h, drying temperature 105
DEG C, drying time 6-10h.
Protective gas is any one in nitrogen, argon gas or helium that mass fraction is 99.99% in the step (2)
Kind, the charge flow rate of protective gas is 100-400sccm.
Step (2) the high temperature carburizing temperature be 700-900 DEG C, carbonization time 2-4h, heating rate be 3-6 DEG C/
min。
The mass ratio of iron nitrogen codope carbon sample and activator is 1:(1-3 in the step (3)), activator is nitric acid
Ammonium, ammonium carbonate or ammonium hydrogen carbonate.
Drying temperature is 80-120 DEG C in the step (3), drying time 12-24h；Calcination temperature is 250-350 DEG C,
Calcination time is 1-3h, and heating rate is 2-5 DEG C/min.
The beneficial effects of the present invention are:
(1) it is living that carbon source used by " dumbbell shape " iron nitrogen codope porous carbon of the present invention, iron nitrogen dopant and surface are prepared
Property agent be easy obtain, it is cheap, be advantageously implemented large-scale production；
(2) it is porous to prepare the nitrogen codope of " dumbbell shape " iron for the method that the present invention uses hydro-thermal method, carbonizatin method and activation method to combine
Carbon, technique and simple flow, easily controllable, sustainability is strong, generates in operating process without pollutants such as soda acids, products obtained therefrom matter
It measures；
(3) " dumbbell shape " iron nitrogen codope porous carbon produced by the present invention, conductive height, specific surface area and pore volume can
The advantages that tune, iron nitrogen content is controllable, is conducive to the optimization that its physical and chemical performance is realized by the regulation to its structure；
(4) " dumbbell shape " iron nitrogen codope porous carbon produced by the present invention is carried in electrode material, separation, absorption, sensing, catalyst
There is potential application value in the fields such as body and gas storage, the quick hair for China's Novel Carbon Nanomaterials that can make greater efforts to promote
Exhibition.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
Fig. 2 is the transmission electron microscope picture for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
Fig. 3 is the XRD diagram for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
Fig. 4 is the Raman spectrogram for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
Fig. 5 is the XPS figure for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
The high-resolution XPS figure that Fig. 6 is the Fe 2p for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains；
The high-resolution XPS figure that Fig. 7 is the N 1s for " dumbbell shape " iron nitrogen codope porous carbon that the embodiment of the present invention 1 obtains.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, steps are as follows:
(1) glucose, six ferrous sulfate hydrate ammoniums and the neopelex deionized water for being 20:1:1 by mass ratio
Dissolution, the stir process on magnetic stirring apparatus, mixing time 10min, stirring rate 200r/min, after to be put into ultrasonic wave clear
It washes and carries out ultrasound in device, then ultrasonic time 1h, ultrasonic power 100W are transferred to the stainless steel hydro-thermal of polytetrafluoroethyllining lining
Reaction kettle carries out hydro-thermal reaction, and hydrothermal temperature is 180 DEG C, and the hydro-thermal time is 15h, is cooled to room temperature rear resulting material and spends
Ionized water filtration washing is put into drying in oven, drying temperature is 105 DEG C, drying time 6h, obtains hydro-thermal carbon sample to neutrality
Product；
(2) the hydro-thermal carbon sample that step (1) obtains is put into tube furnace, the nitrogen high temperature carbon for being 99.99% in mass fraction
Change processing, charge flow rate 100sccm, carburizing temperature are 800 DEG C, carbonization time 4h, and heating rate is 3 DEG C/min, is obtained
Iron nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with mass ratio for 1:1 with ammonium nitrate, the bodies such as addition
It after long-pending alcohol and water dissolution, is put into baking oven and is dried, drying temperature is 80 DEG C, and drying time is that for 24 hours, then will dry
Product is calcined in nitrogen gas atmosphere, and calcination temperature is 250 DEG C, calcination time 3h, and heating rate is 2 DEG C/min,
Taking-up is washed with deionized water, and dry 12h at 120 DEG C, obtains " dumbbell shape " iron nitrogen codope porous carbon in baking oven.
Fig. 1 and Fig. 2 is the scanning electron microscope (SEM) photograph and transmission electron microscope picture of " dumbbell shape " iron nitrogen codope porous carbon of preparation, we
It should be apparent that gained sample is the carbon ball of typical " dumbbell shape " structure, about hundreds of nanometers of the diameter of ball.Fig. 3's
It can be seen that two distant diffraction maximums, respectively correspond (002) and (100) crystal face of graphite, illustrate sample in XRD diagram
Mainly undefined structure, degree of graphitization be not high；The presence at the peak D shows that gained " dumbbell shape " iron nitrogen codope is porous in Fig. 4
Carbon surface there are some defects, these defects may be carbon material surface hole and functional group caused by；The presence at the peak G shows
The good conductivity of gained " dumbbell shape " iron nitrogen codope porous carbon, and the peak value at the peak G is greater than the peak D, shows it with certain stone
Mo Huadu.The XPS of " dumbbell shape " iron nitrogen codope porous carbon that Fig. 5 is schemes, Fig. 6 and Fig. 7 be respectively corresponding Fe 2p and
The high-resolution XPS of N 1s schemes, and shows that we enter iron and nitrogen-doping in carbon sample, and measure the atom of C, O, Fe, N
Percentage is respectively 80.92,18.01,0.15 and 0.91at%.In conclusion the present invention has been successfully prepared a kind of " dumbbell shape "
Iron nitrogen codope porous carbon materials.
Embodiment 2
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, steps are as follows:
(1) sucrose, six ferrous sulfate hydrate ammoniums and the dodecyl sodium sulfate deionized water dissolving for being 25:2:1 by mass ratio,
The stir process on magnetic stirring apparatus, mixing time 20min, stirring rate 150r/min, after be put into ultrasonic cleaner
Middle progress ultrasound, then ultrasonic time 2h, ultrasonic power 150W are transferred to the stainless steel water thermal response of polytetrafluoroethyllining lining
Kettle carries out hydro-thermal reaction, and hydrothermal temperature is 180 DEG C, and the hydro-thermal time is 13h, is cooled to room temperature rear resulting material deionization
Water filtration washing is put into drying in oven, drying temperature is 105 DEG C, drying time 8h, obtains hydro-thermal carbon sample to neutrality；
(2) the hydro-thermal carbon sample that step (1) obtains is put into tube furnace, the helium high temperature carbon for being 99.99% in mass fraction
Change processing, charge flow rate 200sccm, carburizing temperature are 800 DEG C, carbonization time 3h, and heating rate is 5 DEG C/min, is obtained
Iron nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with mass ratio for 1:2 with ammonium carbonate, the bodies such as addition
It after long-pending alcohol and water dissolution, is put into baking oven and is dried, drying temperature is 100 DEG C, then drying time 18h will be done
Dry product is calcined in nitrogen gas atmosphere, calcination temperature be 300 DEG C, calcination time 2h, heating rate be 3 DEG C/
Min, taking-up are washed with deionized water, and dry 16h at 100 DEG C, obtains " dumbbell shape " iron nitrogen codope porous carbon in baking oven.
Embodiment 3
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, steps are as follows:
(1) glycogen, six ferrous sulfate hydrate ammoniums and the dodecyl sodium sulfate deionized water dissolving for being 30:3:1 by mass ratio,
The stir process on magnetic stirring apparatus, mixing time 30min, stirring rate 100r/min, after be put into ultrasonic cleaner
Middle progress ultrasound, then ultrasonic time 3h, ultrasonic power 300W are transferred to the stainless steel water thermal response of polytetrafluoroethyllining lining
Kettle carries out hydro-thermal reaction, and hydrothermal temperature is 190 DEG C, and the hydro-thermal time is 10h, is cooled to room temperature rear resulting material deionization
Water filtration washing is put into drying in oven, drying temperature is 105 DEG C, drying time 10h, obtains hydro-thermal carbon sample to neutrality；
(2) the hydro-thermal carbon sample that step (1) obtains is put into tube furnace, the argon gas high temperature carbon for being 99.99% in mass fraction
Change processing, charge flow rate 400sccm, carburizing temperature are 900 DEG C, carbonization time 2h, and heating rate is 6 DEG C/min, is obtained
Iron nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with mass ratio for 1:3 with ammonium hydrogen carbonate, be added etc.
It after alcohol and the water dissolution of volume, is put into baking oven and is dried, drying temperature is 120 DEG C, drying time 12h, then will
Desciccate is calcined in nitrogen gas atmosphere, calcination temperature be 350 DEG C, calcination time 1h, heating rate be 5 DEG C/
Min, taking-up are washed with deionized water, and drying for 24 hours, obtains " dumbbell shape " iron nitrogen codope porous carbon at 80 DEG C in baking oven.
Embodiment 4
A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, steps are as follows:
(1) mass ratio is molten for the cellulose, six ferrous sulfate hydrate ammoniums and dodecyl sodium sulfate deionized water of 25:2:1
Solution, the stir process on magnetic stirring apparatus, mixing time 25min, stirring rate 150r/min, after be put into ultrasonic cleaning
Ultrasonic, ultrasonic time 2h, ultrasonic power 200W are carried out in device, the stainless steel hydro-thermal for being then transferred to polytetrafluoroethyllining lining is anti-
Answer kettle carry out hydro-thermal reaction, hydrothermal temperature be 160 DEG C, the hydro-thermal time be 14h, be cooled to room temperature rear resulting material spend from
Sub- water filtration washing is put into drying in oven, drying temperature is 105 DEG C, drying time 8h, obtains hydro-thermal carbon sample to neutrality
Product；
(2) the hydro-thermal carbon sample that step (1) obtains is put into tube furnace, the nitrogen high temperature carbon for being 99.99% in mass fraction
Change processing, charge flow rate 200sccm, carburizing temperature are 700 DEG C, carbonization time 3h, and heating rate is 4 DEG C/min, is obtained
Iron nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with mass ratio for 1:2 with ammonium carbonate, the bodies such as addition
It after long-pending alcohol and water dissolution, is put into baking oven and is dried, drying temperature is 100 DEG C, then drying time 18h will be done
Dry product is calcined in nitrogen gas atmosphere, calcination temperature be 300 DEG C, calcination time 2h, heating rate be 4 DEG C/
Min, taking-up are washed with deionized water, and dry 12h at 120 DEG C, obtains " dumbbell shape " iron nitrogen codope porous carbon in baking oven.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon, it is characterised in that steps are as follows:
(1) by carbon source, iron nitrogen dopant and surfactant deionized water dissolving, ultrasonic cleaning is put into after stir process
Ultrasound is carried out in device, hydrothermal reaction kettle is transferred to and carries out hydro-thermal reaction, is cooled to room temperature rear resulting material deionized water filtering and is washed
It washs to neutrality, is put into drying in oven, obtain hydro-thermal carbon sample；
(2) hydro-thermal carbon sample in step (1) is put into tube furnace, in protective gas atmosphere high temperature carbonization treatment, obtains iron
Nitrogen codope carbon sample；
(3) the iron nitrogen codope carbon sample that step (2) obtains uniformly is mixed with activator, isometric alcohol and water-soluble is added
Xie Hou is put into baking oven and is dried, and then calcines desciccate in nitrogen gas atmosphere, and deionized water is used in taking-up
It cleans, obtains " dumbbell shape " iron nitrogen codope porous carbon after dry in baking oven.
2. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly carbon source is glucose, sucrose, glycogen or cellulose in (1), and iron nitrogen dopant is six ferrous sulfate hydrate ammoniums, surfactant
For neopelex or dodecyl sodium sulfate；The mass ratio of carbon source, iron nitrogen dopant and surfactant is (20-
30): (1-3): 1.
3. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly mixing time is 10-30min, stirring rate 100-200r/min, ultrasonic time 1-3h in (1), and ultrasonic power is
100-300W；Hydrothermal temperature is 160-190 DEG C, and the hydro-thermal time is 10-15h, and drying temperature is 105 DEG C, and drying time is
6-10h。
4. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly protective gas is any one in nitrogen, argon gas or helium that mass fraction is 99.99% in (2), protective gas into
Throughput is 100-400sccm.
5. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly (2) high temperature carburizing temperature is 700-900 DEG C, carbonization time 2-4h, and heating rate is 3-6 DEG C/min.
6. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly the mass ratio of iron nitrogen codope carbon sample and activator is 1:(1-3 in (3)), activator is ammonium nitrate, ammonium carbonate or carbonic acid
Hydrogen ammonium.
7. the preparation method of " dumbbell shape " iron nitrogen codope porous carbon according to claim 1, it is characterised in that: the step
Suddenly drying temperature is 80-120 DEG C in (3), drying time 12-24h；Calcination temperature is 250-350 DEG C, calcination time 1-
3h, heating rate are 2-5 DEG C/min.
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| CN115403041A (en) * | 2022-09-15 | 2022-11-29 | 中国地质大学（北京） | Hemicellulose-based hollow porous carbon, preparation method thereof and application thereof in zinc ion energy storage device |
| CN115490232A (en) * | 2022-11-02 | 2022-12-20 | 江西省科学院应用化学研究所 | Nitrogen-sulfur co-doped or sulfur-doped porous carbon material and preparation method and application thereof |
| CN115779855A (en) * | 2022-10-24 | 2023-03-14 | 广州大学 | Preparation method of hot-process iron-nitrogen co-doped magnetic carbon material |
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