CN105854801A - Nitrogen-doped porous carbon material and preparation method and application thereof - Google Patents
Nitrogen-doped porous carbon material and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/504—Carbon dioxide
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention provides a nitrogen-doped porous carbon material and a preparation method and application thereof. The preparation method includes steps: weighing ethylene diamine tetraacetic acid metal salt, putting in a nickel crucible, placing in a high-temperature quartz tubular furnace, performing high-temperature pyrolysis under inert gas protection to obtain a black composite carbon material, immersing the composite carbon material in an acid solution, stirring, washing to neutral, and performing vacuum drying to obtain the nitrogen-doped porous carbon material. The nitrogen-doped porous carbon material prepared according to the method has excellent CO2 adsorption performance and stability and has a potential to serve as a commercial adsorbent.
Description
Technical field
The invention belongs to porous carbon materials preparation field, porous carbon materials being specifically related to a kind of N doping and preparation method thereof and use
On the way.
Background technology
Fossil fuel is depended on unduly and be result in CO by the mankind2Be a large amount of discharges of main greenhouse gases, and cause global warming,
A series of environment and the ecological problems such as sea level rise, Melting Glaciers and snow line rising, have begun to the agricultural to human society,
The field such as the energy, politics.Therefore, CO the most feasible, with low cost is developed2Capture material and technology are significant.
At present, CO2Separate method for catching and mainly have solvent absorption, membrane separation process, low temperature processing and absorption method.These sides
In method, absorption method is most to have large-scale application owing to it has the advantages such as technique is simple, energy consumption is less, corrosivity is low
The material of potentiality.It is presently used for CO2The material of absorption mainly has zeolite molecular sieve, clay, carbonaceous adsorbent.Porous carbon
Material has that specific surface area is big, pore structure is flourishing, surface easily modified, prepare the advantages such as simple and with low cost, be a kind of non-
The sorbent material of Chang Youxiu, also has great application prospect at other fields such as catalysis, separation, energy storages.It is to CO2
Absorption can be divided into physical absorption and chemisorbed.Physical absorption occurs mainly in micropore, when pore-size distribution is 0.5～1.7
CO relatively it is beneficial to time in the range of nm2Absorption, specific surface area and pore volume be weigh physical absorption amount index.Chemisorbed is sent out
Raw on the surface of activated carbon, the functional group of activated carbon surface can with adsorbed material generation chemical reaction thus produce chemisorbed
Effect.
The preparation technology of porous carbon materials mainly has direct carborization and activation method, and the porous carbon that the latter obtains has more preferable permeability
Structure, it is best that activation method is broadly divided into physically activated and chemical activation, the especially activation effect with KOH.But, activation
There are some drawbacks, operating process is proposed higher requirement, if dealt with improperly, easily environment being caused bigger harm on the contrary.
In sum, preparation CO2High-performance absorption porous carbon materials mainly considers morphology control and Heteroatom doping, and mesh
Mostly front method is to be synthesized by multistep, and its operation is complex, is not suitable for industrialization large-scale production.How there is coordination excellent
Change the relation between the selection of nitrogen source, activation control, Heteroatom doping three, prepare practical high-performance CO2Absorption
Agent, has great importance.The present invention utilizes a kind of little molecular precursor, utilizes method that one-step method is pyrolyzed with the chemistry of its uniqueness
Structure can reach the purpose of self-activation and N doping simultaneously.
Summary of the invention
It is an object of the invention to provide the preparation method of the high-performance carbon dioxide absorbing material of a kind of situ Nitrogen Doping, this material is adopted
Be presoma by micromolecular compound tetraacetic acid metal salt, be pyrolyzed by one-step method, utilize molecular structure itself nitrogen and
Inorganic base ion respectively reaches the purpose of N doping and in-situ activation, has high nitrogen doped, big specific surface area, aperture to obtain
The porous carbon materials being evenly distributed, and it is applied to CO2Absorption.
The present invention is achieved through the following technical solutions:
The porous carbon materials of a kind of N doping, the porous carbon materials of described N doping is shaggy block structure, specific surface area
For 2916.64m2/ g, pore volume is 1.627cm3/ g, average pore diameter is 1.68nm；In the porous carbon materials of described N doping,
The mass fraction of nitrogen is 2.58%；Under 273K, the porous carbon materials of described N doping is used for CO2Absorption, adsorbance reaches
Arrive 5.79mmol/g.
A kind of preparation method of the porous carbon materials of N doping, step is as follows:
Weigh tetraacetic acid metal salt and be put in nickel crucible, be placed in high quartz tube furnace, under inert gas is protected, enter
Row high temperature pyrolysis, obtains the complex carbon material of black after pyrolysis, described complex carbon material is immersed in acid solution stirring,
It is washed out to neutrality, vacuum drying, i.e. obtains the porous carbon materials of N doping.
In the present invention, described tetraacetic acid metal salt is EDTA Dipotassium salt, ethylenediaminetetraacetic acid tripotassium salt, second
Edetate disodium salt, the one of tetrasodium salt of EDTA.
In the present invention, described inert gas is N2, the one of Ar；Flow velocity is 20～100mL/min.
In the present invention, the heating rate of described high temperature pyrolysis is 3～8 DEG C/min, and temperature is 650～900 DEG C；Retention time is
0.5～3h.
In the present invention, described diluted acid is HCl, HNO3One, volume fraction is 3～10%, and described mixing time is 0.5～2
h。
In the present invention, described vacuum drying temperature is 60～110 DEG C, and the time is 6～24h.
The porous carbon materials of described N doping is used for CO absorption2。
The present invention uses and contains carboxyl (-COO) and tertiary amine groups (-NR simultaneously3) organic micromolecule compound be precursor, pass through
High temperature pyrolysis method prepares high performance CO2Adsorbent.The invention has the beneficial effects as follows:
(1) material is conveniently easy to get, wide material sources, it is simple to large-scale production and application.
(2) preparation method is simple, strong operability.Material originally can reach the purpose of activation and N doping in pyrolytic process,
Save steps such as extraly material being loaded, be combined, and amount and the pyrolysis temperature of alkali metal ion in molecule can be utilized
Regulate and control with to material behavior.
(3) material prepared by the method has fabulous CO2Absorption property, stability is strong, the potential adsorbent becoming commercialization.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) photograph and the transmission electron microscope picture of the material with carbon element that embodiment 1 prepares, and wherein a is scanning electron microscope (SEM) photograph, and b is
Transmission electron microscope picture；
Fig. 2 is the x-ray photoelectron energy spectrogram of the material with carbon element that embodiment 1 prepares；
Fig. 3 be the material with carbon element for preparing of embodiment 1 under 273K to CO2Adsorption isotherm line chart.
Detailed description of the invention
Below in conjunction with being embodied as example, the present invention will be further described:
Embodiment 1
Weigh 5g EDTA Dipotassium salt and be put in nickel crucible, be placed in high quartz tube furnace at N2Air-flow (20mL/min)
Under protection, it is warming up to 750 DEG C with the heating rate of 3 DEG C/min, maintains natural cooling after 1h, after pyrolysis, obtain black
Complex carbon material, be subsequently adding excess 5%HCl (v/v) solution, make complex carbon material submergence, stir 1h, be washed out
To neutral, 80 DEG C of vacuum drying 12h, i.e. obtain the porous carbon materials of N doping.
Porous carbon materials is applied to CO2The method of absorption is:
By (1) gained porous carbon materials distilled water and dehydrated alcohol mixed liquor (preparing by the volume ratio of 1:1) soaking and washing
After, it is put in the air dry oven of 100 DEG C and is dried 10h, be then put in vacuum drying oven and be dried 2h.One is weighed after cooling
Determine mass charge in adsorption column, carry out CO2Adsorption test, CO in strict control unstripped gas2Concentration about 10%, raw material
Throughput is at 0.1L min-1Under conditions of, and record the adsorption breakthrough curve of porous carbon materials and the CO of activated carbon2Adsorbance.
By Fig. 1 (a) it can be seen that this material is bulk, find out that its outer surface is the most coarse from high power scanning electron microscope, pass through
Fig. 1 (b) can be seen that material is covered with loose structure.Further, according to nitrogen adsorption-desorption isotherm, the BET of this material
Specific surface area is 2916.64m2/ g, pore volume is 1.627cm3/ g, wherein, the micropore specific area calculated according to t-plot method
For 2156.13m2/ g, micropore volume is 1.001cm3/ g, average pore diameter is 1.68nm.From x-ray photoelectron energy spectrogram (figure
2) it can be seen that in material carbon account for 91.88%, there is more rich nitrogen content (2.58%).Use it for CO2Absorption
Test result such as Fig. 3, adsorbance reaches 5.79mmol/g (273K), compared to the nitrogen of some high adsorption capacities of report in document
Doped absorbent materials (Energy Environ.Sci., 2014,7,3478), this material possesses fabulous absorption property.
Embodiment 2
Weigh 5g ethylenediaminetetraacetic acid tripotassium salt and be put in nickel crucible, be placed in high quartz tube furnace at Ar air-flow (60mL/min)
Under protection, it is warming up to 650 DEG C with the heating rate of 5 DEG C/min, maintains natural cooling after 3h, after pyrolysis, obtain black
Complex carbon material, be subsequently adding excess 10%HNO3(v/v) solution, makes complex carbon material submergence, stirs 0.5h, then
Washing, 60 DEG C of vacuum drying 24h, i.e. obtain the porous carbon adsorbing material of N doping.
Utilize this material CO absorption2, result shows: the adsorbance of this material is 5.38mmol/g (273K).
Embodiment 3
Weigh 5g disodium EDTA and be put in nickel crucible, be placed in high quartz tube furnace at N2Air-flow (100mL/min)
Under protection, it is warming up to 900 DEG C with the heating rate of 8 DEG C/min, maintains natural cooling after 0.5h, after pyrolysis, obtain black
Complex carbon material, be subsequently adding excess 3%HNO3(v/v) solution, makes complex carbon material submergence, stirs 2h, then washes
Wash to neutrality, 110 DEG C of vacuum drying 6h, i.e. obtain the porous carbon adsorbing material of N doping.
Utilize this material CO absorption2, result shows: the adsorbance of this material is 5.06mmol/g (273K).
Embodiment 4
Weigh 5g tetrasodium salt of EDTA and be put in nickel crucible, be placed in high quartz tube furnace at N2Air-flow (100mL/min)
Under protection, it is warming up to 900 DEG C with the heating rate of 6 DEG C/min, maintains natural cooling after 0.5h, after pyrolysis, obtain black
Complex carbon material, be subsequently adding excess 5%HCl (v/v) solution, make complex carbon material submergence, stir 2h, be washed out
To neutral, 110 DEG C of vacuum drying 6h, i.e. obtain the porous carbon adsorbing material of N doping.
Utilize this material CO absorption2, result shows: the adsorbance of this material is 4.87mmol/g (273K).
Each raw material cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize this
Invention, embodiment numerous to list herein.The bound value of the technological parameter of the present invention, interval value can realize the present invention,
Embodiment numerous to list herein.Therefore, under the general concept limited without departing substantially from claim and equivalency range, the present invention is also
It is not limited to specific details and shown here as the legend with description.
Claims (8)
1. the porous carbon materials of a N doping, it is characterised in that the porous carbon materials of described N doping is shaggy bulk
Structure, specific surface area is 2916.64m2/ g, pore volume is 1.627cm3/ g, average pore diameter is 1.68nm；Described N doping
Porous carbon materials in, the mass fraction of nitrogen is 2.58%；Under 273K, the porous carbon materials of described N doping is used for CO2
Absorption, adsorbance has reached 5.79mmol/g.
2. the preparation method of the porous carbon materials of a N doping, it is characterised in that step is as follows:
Weigh tetraacetic acid metal salt and be put in nickel crucible, be placed in high quartz tube furnace, under inert gas is protected, enter
Row high temperature pyrolysis, obtains the complex carbon material of black after pyrolysis, described complex carbon material is immersed in acid solution stirring,
It is washed out to neutrality, vacuum drying, i.e. obtains the porous carbon materials of N doping.
The preparation method of the porous carbon materials of a kind of N doping the most according to claim 2, it is characterised in that described second two
Amine tetraacethyl slaine is EDTA Dipotassium salt, ethylenediaminetetraacetic acid tripotassium salt, disodium EDTA, second two
The one of amine tetraacethyl tetrasodium salt.
The preparation method of the porous carbon materials of a kind of N doping the most according to claim 2, it is characterised in that described is lazy
Property air-flow is N2, the one of Ar；Flow velocity is 20～100mL/min.
The preparation method of the porous carbon materials of a kind of N doping the most according to claim 2, it is characterised in that described height
The heating rate that warm solves is 3～8 DEG C/min, and temperature is 650～900 DEG C；Retention time is 0.5～3h.
The preparation method of the porous carbon materials of a kind of N doping the most according to claim 2, it is characterised in that described is dilute
Acid is HCl, HNO3One, volume fraction is 3～10%, and described mixing time is 0.5～2h.
The preparation method of the porous carbon materials of a kind of N doping the most according to claim 2, it is characterised in that described is true
Empty baking temperature is 60～110 DEG C, and the time is 6～24h.
8. the porous carbon of N doping prepared by the preparation method of the porous carbon materials of the N doping described in claim 2～7 any one
The purposes of material, it is characterised in that the porous carbon materials of described N doping is used for CO absorption2。
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Cited By (11)
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|---|---|---|---|---|
| CN106423276A (en) * | 2016-09-13 | 2017-02-22 | 合肥工业大学 | Preparation method of nickel electric Fenton catalyst supported by nitrogen mixed with carbon |
| CN106862589A (en) * | 2017-02-15 | 2017-06-20 | 珠海市吉林大学无机合成与制备化学重点实验室 | Metallic nickel nitrogen-doped porous carbon material, preparation method and applications |
| CN107068423A (en) * | 2017-04-24 | 2017-08-18 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
| CN109107596A (en) * | 2018-08-20 | 2019-01-01 | 河南师范大学 | The preparation method of the carbon nano enzyme of active metal and nitrogen codope and its application that hydrogen peroxide is detected as nanometer bio probe |
| CN109133030A (en) * | 2018-09-25 | 2019-01-04 | 桂林电子科技大学 | A kind of preparation method and applications of nitrogen-doped porous carbon material |
| CN109264713A (en) * | 2018-09-20 | 2019-01-25 | 中国科学院广州能源研究所 | A kind of preparation method of the carbon dioxide physical absorption surface area porous carbon of biomass coke tar base-height ratio |
| CN109767929A (en) * | 2019-03-21 | 2019-05-17 | 北京理工大学 | Porous carbon electrodes derived from a kind of organic salt |
| CN109908864A (en) * | 2019-03-21 | 2019-06-21 | 浙江师范大学 | A kind of preparation method of N doping porous carbon group carbonic anhydride adsorption agent |
| CN110028069A (en) * | 2019-04-18 | 2019-07-19 | 河南师范大学 | A kind of preparation method of the advanced carbon electrode material of multi-stage porous for supercapacitor |
| CN110078046A (en) * | 2019-05-14 | 2019-08-02 | 江西省科学院应用化学研究所 | A kind of preparation and application of nitrogen-doped porous carbon material |
| CN110182800A (en) * | 2019-07-15 | 2019-08-30 | 天津工业大学 | A kind of method for preparation of active carbon based on ethylene diamine tetraacetic acid sylvite |
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| CN106423276B (en) * | 2016-09-13 | 2018-11-06 | 合肥工业大学 | A kind of preparation method of nitrogen-doped carbon nickel-loaded Fenton catalyst |
| CN106423276A (en) * | 2016-09-13 | 2017-02-22 | 合肥工业大学 | Preparation method of nickel electric Fenton catalyst supported by nitrogen mixed with carbon |
| CN106862589A (en) * | 2017-02-15 | 2017-06-20 | 珠海市吉林大学无机合成与制备化学重点实验室 | Metallic nickel nitrogen-doped porous carbon material, preparation method and applications |
| CN107068423B (en) * | 2017-04-24 | 2019-01-08 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
| CN107068423A (en) * | 2017-04-24 | 2017-08-18 | 江苏大学 | A kind of Preparation method and use of cobalt oxide/graphene/multi-stage porous carbon electrode material |
| CN109107596A (en) * | 2018-08-20 | 2019-01-01 | 河南师范大学 | The preparation method of the carbon nano enzyme of active metal and nitrogen codope and its application that hydrogen peroxide is detected as nanometer bio probe |
| CN109264713A (en) * | 2018-09-20 | 2019-01-25 | 中国科学院广州能源研究所 | A kind of preparation method of the carbon dioxide physical absorption surface area porous carbon of biomass coke tar base-height ratio |
| CN109264713B (en) * | 2018-09-20 | 2020-06-12 | 中国科学院广州能源研究所 | Preparation method of biomass tar-based high-specific-surface-area porous carbon for carbon dioxide physical adsorption |
| CN109133030A (en) * | 2018-09-25 | 2019-01-04 | 桂林电子科技大学 | A kind of preparation method and applications of nitrogen-doped porous carbon material |
| CN109767929A (en) * | 2019-03-21 | 2019-05-17 | 北京理工大学 | Porous carbon electrodes derived from a kind of organic salt |
| CN109908864A (en) * | 2019-03-21 | 2019-06-21 | 浙江师范大学 | A kind of preparation method of N doping porous carbon group carbonic anhydride adsorption agent |
| CN110028069A (en) * | 2019-04-18 | 2019-07-19 | 河南师范大学 | A kind of preparation method of the advanced carbon electrode material of multi-stage porous for supercapacitor |
| CN110078046A (en) * | 2019-05-14 | 2019-08-02 | 江西省科学院应用化学研究所 | A kind of preparation and application of nitrogen-doped porous carbon material |
| CN110078046B (en) * | 2019-05-14 | 2020-09-08 | 江西省科学院应用化学研究所 | Preparation and application of nitrogen-doped porous carbon material |
| CN110182800A (en) * | 2019-07-15 | 2019-08-30 | 天津工业大学 | A kind of method for preparation of active carbon based on ethylene diamine tetraacetic acid sylvite |
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