CN110416548A - A kind of preparation method and applications of the two-dimensional structure of N doping porous carbon - Google Patents
A kind of preparation method and applications of the two-dimensional structure of N doping porous carbon Download PDFInfo
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- CN110416548A CN110416548A CN201910752196.2A CN201910752196A CN110416548A CN 110416548 A CN110416548 A CN 110416548A CN 201910752196 A CN201910752196 A CN 201910752196A CN 110416548 A CN110416548 A CN 110416548A
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/42—Alloys based on zinc
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- H—ELECTRICITY
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Abstract
The invention discloses a kind of preparation methods of the two-dimensional structure of N doping porous carbon, comprising the following steps: 2-methylimidazole powder is dissolved in methanol, solution A is formed, is placed in water-bath and stirs；Zn-HMT powder is dissolved in methanol, solution B is formed；Solution B is slowly added into solution A, is placed in water-bath after stirring, product is centrifugated, after ethanol washing, is placed in baking oven and dries to obtain ZIF-8 two-dimensional nano chip architecture；ZIF-8 two-dimensional nano chip architecture powder nitric acid acidwashing after argon gas protection annealing obtains product.The two-dimensional structure of N doping porous carbon prepared by this method can be widely applied to electrochemical energy storage, the fields such as isolation and purification and medicament slow release.
Description
Technical field
The present invention relates to Micron-nano composites synthesis technical fields, and in particular to a kind of metal organic frame (MOFs) is
Presoma obtains the preparation method and applications of the two-dimensional structure of N doping porous carbon in conjunction with argon annealed processing.
Background technique
Metal organic frameworks (MOFs) are passed through covalently by transition metal ions organic ligand different from oxygen-containing, nitrogen etc.
Key or ionic-covalent bonds' Coordinate self-assembly and formed have periodic porous crystalline coordination polymer material, also known as
It is porous to match polymer (porous coordination polymer, PCP).MOFs can by different metal ions with have
Machine ligand complex designs and manufactures the metal organic frame with different pore structures and different physics and chemical characteristic.MOFs
Have the feature that porosity, high-specific surface area, have unsatuated metal active site, pore size can design and duct table
It face can functionalization etc..Catalysis, energy storage and conversion and gas absorption with separate etc. shown in multiple fields it is excellent
Performance., as a kind of multifunctional material, the material for synthesizing MOFs can make lower-cost raw material have low frame close for it
Degree and high thermal stability, these advantages make candidate material of the MOFs as energy and material.Therefore N doping prepared by the present invention
The two-dimensional structure of porous carbon combines the bigger serface of porous carbon, provides the active sites of more storage potassium ions, potassium from
Effective buffer function is played to the volume expansion of material during the insertion and abjection of son；N doping brings a large amount of crystal
Defect contributes higher specific capacity.The application field for having further expanded MOFs material makes Large ratio surface, the Gao Kong of MOF material
Gap rate and modifiability these design features are given full play to, and have very big practical utility value.
Summary of the invention
It is an object of the invention to: provide a kind of preparation method of the two-dimensional structure of N doping porous carbon, it is intended to which exploitation is answered
Electrode material for high-performance kalium ion battery.Material preparation method is simple, at low cost, is with a wide range of applications.
To achieve the goals above, the invention provides the following technical scheme:
A kind of preparation method of the two-dimensional structure of N doping porous carbon, comprising the following steps:
(1) 2-methylimidazole powder is dissolved in methanol, forms solution A, is placed in water-bath and stirs；
(2) Zn-HMT powder is dissolved in methanol, forms solution B；
(3) solution B is slowly added into solution A, is placed in water-bath after stirring, product is centrifugated, ethyl alcohol is used
It after washing, is placed in baking oven and dries, obtain ZIF-8 two-dimensional structure；
(4) for ZIF-8 two-dimensional structure powder by argon gas protection annealing, the two-dimensional structure for obtaining N doping porous carbon (may
Containing zinc)；
(5) two-dimensional material of N doping porous carbon (may contain zinc) is placed in nitric acid solution, is stirred to react in water-bath
Product is centrifugated afterwards, then clean with ethanol washing, is placed in baking oven after drying, obtains the two dimension of pure N doping porous carbon
Structure.
Preferably, in step (1), the concentration of 2-methylimidazole is 0.974mol L in solution A-1, temperature in water-bath
It is 30 DEG C；
Preferably, in step (2), the concentration of solution B is 1.828g L-1。
Preferably, in step (3), the temperature in water-bath is 30 DEG C, mixing time 15min；The temperature of baking oven is 75-
85℃。
Preferably, in step (4), annealing temperature is 900 DEG C, and soaking time is 2 hours；
Preferably, in step (5), the volume ratio of concentrated nitric acid and water is 1:2 in nitric acid solution.
Preferably, in step (5), bath temperature is 75-85 DEG C, water bath time 23-25h.
Preferably, in step (5), the temperature of baking oven is 75-85 DEG C.
Further, the two-dimensional structure of prepared N doping porous carbon can be used in the cathode of high-performance kalium ion battery
Material.
Compared with prior art, the present invention its advantageous effects is shown:
1, the two-dimensional structure of N doping porous carbon prepared by the present invention, on the one hand realizes metal ion and specific MOF
Material forms composite construction, then handles to obtain the structure of porous carbon by high-temperature calcination, has given full play to MOF material Large ratio surface
Product, high porosity and modifiable design feature.On the other hand, porous carbon materials not only itself have high specific surface area,
The conduction of porous carbon materials not only can be enhanced by N doping porous carbon in excellent electron transfer rate and good stability
Property reduces the physical properties such as its valence band, but also can increase its surface wetting capability, improve its catalytic activity and adsorption capacity
Etc. chemical property, further increase its chemical property, this preparation also for the two-dimensional structure of N doping porous carbon provides one
A new method；
2, the ZIF-8 of conventional method synthesis is full particle structure, and the present invention successfully prepares two-dimensional sheet structure
ZIF-8, and preparation method of the invention is simple to operation, safety non-pollution is low in cost.
3, the two-dimensional structure of N doping porous carbon prepared by the present invention can be applied to electrochemical energy storage, separation with it is pure
The fields such as change and medicament slow release.
Detailed description of the invention
The FESEM figure that Fig. 1 is Zn-HMT prepared by embodiment 1.
Fig. 2 is the FESEM figure and TEM figure of ZIF-8 two-dimensional nano chip architecture prepared by embodiment 2.
Fig. 3 is FESEM and the TEM figure of the two-dimensional structure of N doping porous carbon prepared by embodiment 2.
Fig. 4 is the XRD diagram of ZIF-8 two-dimensional nano chip architecture prepared by embodiment 2.
Fig. 5 is the chemical property figure of the two-dimensional structure of N doping porous carbon prepared by embodiment 3.
Specific embodiment
For the ease of those skilled in the art's understanding, the present invention will be described with reference to the accompanying drawings and examples.
The preparation of embodiment 1, Zn-HMT powder
(1) zinc nitrate hexahydrate of 4.24g is dissolved in the ethyl alcohol of 30ml and forms solution A, by 1.0g hexamethylenetetramine
Be added in the ethyl alcohol of 50ml, at room temperature stirring until all dissolution form solution B, solution A is added in solution B, in room
15min is persistently stirred to react under temperature；
(2) product is centrifugated respectively, with ethanol washing it is clean after, be placed in 80 DEG C of baking ovens and dry, obtain zinc-six times
Tetramine powder, abbreviation Zn-HMT powder.
Fig. 1 be Zn-HMT manufactured in the present embodiment FESEM scheme, nanometer sheet with a thickness of 10-20 nanometers.
The preparation (1) of the two-dimensional structure of embodiment 2, ZIF-8 two-dimensional nano chip architecture and N doping porous carbon is by 4.0g 2-
Methylimidazole is dissolved in the methanol of 50ml, forms solution A, stirs in 30 DEG C of water-bath, and 0.0366g Zn-HMT powder is molten
Solution B is formed in 20ml methanol, solution B is poured into solution A, is stirred to react 15min in 30 DEG C of water-bath.
(2) product is centrifugated, with ethanol washing it is clean after, be placed in 80 DEG C of baking ovens and dry, obtain ZIF-8 two dimension knot
Structure.
(3) ZIF-8 two-dimensional structure is subjected to 900 DEG C of argon annealeds, the pickling in nitric acid solution is stirred under the conditions of 80 DEG C
For 24 hours, product is centrifugated, with ethanol washing 3 times, then place the product in drying in 80 DEG C of baking ovens, it is porous obtains N doping
The two-dimensional structure of carbon.
Fig. 2 is that the FESEM and TEM of ZIF-8 two-dimensional structure manufactured in the present embodiment scheme.Fig. 3 is nitrogen manufactured in the present embodiment
Adulterate FESEM and the TEM figure of 900 DEG C of two-dimensional structures of porous carbon.It can be found that original nanometer sheet is converted into a large amount of particle, formed
Two-dimensional structure.Fig. 4 is the XRD diagram of two-dimensional sheet ZIF-8 structure manufactured in the present embodiment, corresponding 2 θ is respectively 7.48 °,
It is 10.52 °, 12.84 °, 14.92 °, 16.60 ° and 18.12 °, corresponding with standard peak position reported in the literature, illustrate Zn-HMT at
Function is converted into ZIF-8 crystal.
Embodiment 3, N doping porous carbon two-dimensional structure performance test
(1) two-dimensional structure of N doping porous carbon is uniformly mixed with conductive black and PVDF according to mass ratio 7:1:2
It is dissolved in 1-Methyl-2-Pyrrolidone (NMP), slurries is made, are then evenly applied in copper foil current collector, be placed in 60 DEG C of vacuum
It is dried for 24 hours in drying box.
(2) working electrode is made in the copper foil current collector slice after drying, glass fibre is diaphragm, and electrolyte is binary electricity
Liquid is solved, 2032 button cells are assembled into the glove box full of argon gas, test voltage range is 0.01V-3V vs K+/K。
Fig. 5 is the two-dimensional structure potassium electrochemical storage potassium ion performance map of N doping porous carbon prepared by embodiment 3.It can be with
Find out that the potassium electrical property of the two-dimensional structure of N doping porous carbon is preferable.
Above embodiments are the more typical embodiments of the present invention, not any limitation of the invention, for example, instead
Answer concentration, in the reaction time, bath temperature, annealing temperature etc. all can adjust further.Therefore, general thought according to the present invention,
What technological parameter described in affiliated those skilled in the art was adjusted and was modified, as long as it does not deviate from the concept of invention or
Person beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (9)
1. a kind of preparation method of the two-dimensional structure of N doping porous carbon, the following steps are included:
(1) 2-methylimidazole powder is dissolved in methanol, forms solution A, is placed in water-bath and stirs；
(2) Zn-HMT powder is dissolved in methanol, forms solution B；
(3) solution B is slowly added into solution A, is placed in water-bath after stirring, product is centrifugated, ethanol washing is used
Afterwards, it is placed in baking oven and dries, obtain ZIF-8 two-dimensional nano chip architecture；
(4) ZIF-8 two-dimensional nano chip architecture powder obtains the two-dimensional nano piece knot of N doping porous carbon by argon gas protection annealing
Structure；
(5) the two-dimensional nano sheet material of N doping porous carbon is placed in nitric acid solution, by product after being stirred to react in water-bath
Centrifuge separation, then it is clean with ethanol washing, it is placed in baking oven after drying, obtains the two-dimensional nano piece knot of pure N doping porous carbon
Structure.
2. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (1)
In, the concentration of 2-methylimidazole is 0.974mol L in solution A-1, the temperature in water-bath is 30 DEG C.
3. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (2)
In, the concentration of solution B is 1.828g L-1。
4. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (3)
In, the temperature in water-bath is 30 DEG C, mixing time 15min；The temperature of baking oven is 75-85 DEG C.
5. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (4)
In, annealing temperature is 900 DEG C, and soaking time is 2 hours.
6. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (5)
In, the volume ratio of concentrated nitric acid and water is 1:2 in nitric acid solution.
7. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (5)
In, bath temperature is 75-85 DEG C, water bath time 23-25h.
8. the preparation method of the two-dimensional structure of N doping porous carbon according to claim 1, which is characterized in that step (5)
In, the temperature of baking oven is 75-85 DEG C.
9. the application of the two-dimensional structure of N doping porous carbon, feature as prepared by the method for any one of claim 1-8 exist
In negative electrode material for high-performance kalium ion battery.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111326745A (en) * | 2020-02-12 | 2020-06-23 | 北京化工大学 | Two-dimensional zinc monoatomic/carbon nitrogen composite material and preparation method and application thereof |
| CN111533124A (en) * | 2020-05-12 | 2020-08-14 | 湖南鑫恒环境科技有限公司 | Two-dimensional nitrogen-doped nano porous carbon material and preparation method thereof |
| CN111916736A (en) * | 2020-08-11 | 2020-11-10 | 合肥工业大学 | Preparation method and application of porous carbon with two-dimensional core-shell structure |
| CN112138697A (en) * | 2020-09-14 | 2020-12-29 | 广州大学 | Preparation method and application of manganese-nitrogen co-doped carbon nanosheet electrocatalyst |
| CN112642457A (en) * | 2020-12-21 | 2021-04-13 | 安徽师范大学 | Hollow iron-based metal organic framework material, iron-doped carbon-nitrogen nano material and preparation method |
| CN114057183A (en) * | 2021-11-22 | 2022-02-18 | 合肥工业大学 | Preparation method of nitrogen-doped dendritic porous carbon nanotube |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111326745A (en) * | 2020-02-12 | 2020-06-23 | 北京化工大学 | Two-dimensional zinc monoatomic/carbon nitrogen composite material and preparation method and application thereof |
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| CN111533124A (en) * | 2020-05-12 | 2020-08-14 | 湖南鑫恒环境科技有限公司 | Two-dimensional nitrogen-doped nano porous carbon material and preparation method thereof |
| CN111916736A (en) * | 2020-08-11 | 2020-11-10 | 合肥工业大学 | Preparation method and application of porous carbon with two-dimensional core-shell structure |
| CN111916736B (en) * | 2020-08-11 | 2023-03-17 | 合肥工业大学 | Preparation method and application of porous carbon with two-dimensional core-shell structure |
| CN112138697A (en) * | 2020-09-14 | 2020-12-29 | 广州大学 | Preparation method and application of manganese-nitrogen co-doped carbon nanosheet electrocatalyst |
| CN112138697B (en) * | 2020-09-14 | 2022-12-20 | 广州大学 | Preparation method and application of manganese-nitrogen co-doped carbon nanosheet electrocatalyst |
| CN112642457A (en) * | 2020-12-21 | 2021-04-13 | 安徽师范大学 | Hollow iron-based metal organic framework material, iron-doped carbon-nitrogen nano material and preparation method |
| CN112642457B (en) * | 2020-12-21 | 2022-07-08 | 安徽师范大学 | Hollow iron-based metal organic framework material, iron-doped carbon-nitrogen nano material and preparation method |
| CN114057183A (en) * | 2021-11-22 | 2022-02-18 | 合肥工业大学 | Preparation method of nitrogen-doped dendritic porous carbon nanotube |
| CN114057183B (en) * | 2021-11-22 | 2022-08-26 | 合肥工业大学 | Preparation method of nitrogen-doped dendritic porous carbon nanotube |
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