CN106268636A - Carbon nano-fiber adsorbing material of aminated carbon nano tube doping and preparation method thereof - Google Patents
Carbon nano-fiber adsorbing material of aminated carbon nano tube doping and preparation method thereof Download PDFInfo
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- CN106268636A CN106268636A CN201610664022.7A CN201610664022A CN106268636A CN 106268636 A CN106268636 A CN 106268636A CN 201610664022 A CN201610664022 A CN 201610664022A CN 106268636 A CN106268636 A CN 106268636A
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- Prior art keywords
- carbon nano
- nano tube
- aminated
- aminated carbon
- adsorbing material
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 239000000463 material Substances 0.000 title claims abstract description 98
- 239000002134 carbon nanofiber Substances 0.000 title claims abstract description 55
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002121 nanofiber Substances 0.000 claims abstract description 34
- 238000001523 electrospinning Methods 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 238000003763 carbonization Methods 0.000 claims abstract description 27
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 26
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000009987 spinning Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000004642 Polyimide Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 4
- 229920002480 polybenzimidazole Polymers 0.000 claims description 4
- 229920001721 polyimide Polymers 0.000 claims description 4
- 229920000128 polypyrrole Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052724 xenon Inorganic materials 0.000 claims description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005576 amination reaction Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001913 cellulose Substances 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910052743 krypton Inorganic materials 0.000 claims description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002048 multi walled nanotube Substances 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002041 carbon nanotube Substances 0.000 claims 1
- 229910021393 carbon nanotube Inorganic materials 0.000 claims 1
- 229920002301 cellulose acetate Polymers 0.000 claims 1
- QEWYKACRFQMRMB-UHFFFAOYSA-N fluoroacetic acid Chemical compound OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims 1
- 239000011261 inert gas Substances 0.000 claims 1
- 239000002070 nanowire Substances 0.000 claims 1
- -1 polybenzoxazine Polymers 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 30
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 25
- 229960004424 carbon dioxide Drugs 0.000 abstract description 16
- 239000001569 carbon dioxide Substances 0.000 abstract description 13
- 238000001179 sorption measurement Methods 0.000 abstract description 13
- 238000003756 stirring Methods 0.000 abstract description 11
- 235000011089 carbon dioxide Nutrition 0.000 abstract description 2
- 238000005304 joining Methods 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000006253 efflorescence Methods 0.000 description 4
- 206010037844 rash Diseases 0.000 description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 229920000767 polyaniline Polymers 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 description 2
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
-
- 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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- 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
-
- 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
- B01J20/28014—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 form
- B01J20/28023—Fibres or filaments
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Fibers (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides the preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, it is characterized in that, including: the first step: at room temperature, first by aminated carbon nano tube ultrasonic disperse 1～10h in a solvent, then the precursor polymer of carbon nano-fiber is added in above-mentioned dispersion liquid and stir to being completely dissolved, obtain the electrospinning raw material that mass fraction is 5～30%；Second step: the electrospinning raw material first step obtained joins in electrostatic spinning apparatus, carries out electrostatic spinning, obtains the Hybrid nanofibers material containing aminated carbon nano tube；3rd step: the Hybrid nanofibers material containing aminated carbon nano tube prepared by second step carries out carbonization treatment, it is thus achieved that the carbon nano-fiber adsorbing material of aminated carbon nano tube doping.The carbon nano-fiber adsorbing material that the present invention is obtained has preferable adsorption capacity, higher selectivity and cyclical stability to carbon dioxide, can meet the collecting carbonic anhydride needs in different discharge place.
Description
Technical field
The present invention relates to carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping and preparation method thereof, belong to
Carbon dioxide adsorption technical field.
Background technology
The a large amount of use of Fossil fuel causes the gas concentration lwevel in air to increase year by year, cause greenhouse effect to highlight,
A series of environment such as the rising of earth surface temperature, Melting Glaciers, sea-level rise, Extreme Weather Events frequently generation are asked with ecology
Topic, therefore trapping and the storage of carbon dioxide is extremely important.Adsorption capacity is big, selectivity owing to having for absorption method
The advantages such as high, energy consumption is low and easily separated and receive significant attention, become collecting carbonic anhydride and field of storage study hotspot it
One.Porous active Carbon Materials has that specific surface area is high, pore structure abundant, chemical property and the advantage such as macroscopic property is stable, is
A kind of conventional carbon dioxide adsorption separation solid absorbent.But pure material with carbon element is mainly thing to the adsorption of carbon dioxide
Reason absorption, causes its carbon dioxide adsorption and selectivity the most poor.Amine substance is used to be modified material with carbon element improving
The carbon dioxide adsorption selectivity of material, as disclosed in domestic patent CN105289530A " a kind of based on ordered mesopore carbon two
Carbonoxide adsorbent and preparation method ", this material is, by infusion process, polymine loads to improve on material with carbon element suction
Attached selectivity, but the load of polymine significantly reduces specific surface area and the porosity of material with carbon element.Additionally, existing granule
The most generally there is the problem of easy efflorescence in shape material with carbon element, limits its operability and practical application energy.Carbon is received
The structural advantages such as rice fibrous material is good with its seriality, pore passage structure is abundant, can effectively overcome granular materials not connect because of its structure
The applied defect that continuous property and easy efflorescence are brought, shows huge application potential, but how to improve in adsorbing separation field
The carbon dioxide adsorption selectivity of carbon nano-fiber and mechanical performance are still a difficult problem urgently to be resolved hurrily.
Summary of the invention
It is an object of the invention to provide the preparation side of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping
Method, to solve carbon nano-fiber adsorptive selectivity difference and the material with carbon element problem that the most generally there is easy efflorescence.
In order to achieve the above object, the invention provides the carbon nano-fiber adsorption material of a kind of aminated carbon nano tube doping
The preparation method of material, it is characterised in that including:
The first step: at room temperature, first by aminated carbon nano tube ultrasonic disperse 1～10h in a solvent, then receives carbon
The precursor polymer of rice fiber is added in above-mentioned dispersion liquid and is stirred to being completely dissolved, and obtaining mass fraction is 5～30%
Electrospinning raw material；
Second step: the electrospinning raw material first step obtained joins in electrostatic spinning apparatus, carries out electrostatic spinning, is contained
The Hybrid nanofibers material of aminated carbon nano tube；
3rd step: the Hybrid nanofibers material containing aminated carbon nano tube prepared by second step carries out carbonization treatment,
Obtain the carbon nano-fiber adsorbing material of aminated carbon nano tube doping.
Preferably, described electrospinning conditions is: electrostatic pressure is 10～40kV, and syringe pump flow velocity is 0.3～4mL/h,
Spinning head is 6～20cm away from receiving screen distance.
Preferably, the supersonic frequency that the ultrasonic disperse in the described first step uses is 20～25kHz.
Preferably, described aminated carbon nano tube is amination multi-walled carbon nano-tubes, external diameter 8～15nm, internal diameter 2～
4nm, length 0.5～55 μm, specific surface area ＞ 233m2/ g, aminated carbon nano tube mass fraction in electrospinning raw material is 0.5
～5%.
Preferably, described solvent is the solvent dissolving precursor polymer.
It is highly preferred that described solvent be DMF, Methanamide, oxolane, N-Methyl pyrrolidone,
Chloroform, N,N-dimethylacetamide, methanol, ethanol, water, acetone, dichloromethane, formic acid, acetic acid, dimethyl sulfoxide, ether, three
One or more mixture in monoxone, trifluoroacetic acid and pyridine.
Preferably, described precursor polymer be polyacrylonitrile, polyimides, polyvinyl butyral resin, polyphenyl also
Piperazine, polyaniline, polypyrrole, polybenzimidazoles, phenolic resin, polyvinylpyrrolidone, polyvinyl alcohol, cellulose, acetate fiber
One or more mixture in element and ethyl cellulose.
Preferably, described carbonization treatment includes: is first warming up to 150～300 DEG C in air atmosphere and carries out at pre-oxidation
Reason 0.5～5h, is warming up to 600～1600 DEG C under protective gas is protected afterwards, carries out carbonization treatment 0.5～20h, drop subsequently
Temperature.
It is highly preferred that described protective gas is one or more in nitrogen, helium, neon, argon, Krypton, xenon
Combination.
Present invention also offers the carbon nano-fiber adsorbing material that the aminated carbon nano tube prepared by said method adulterates.
Compared with prior art advantages of the present invention is as follows:
Present invention process is simple, by carbon nano-fiber surface and interface doping aminated carbon nano tube, it is thus achieved that can be used for
The carbon nano-fiber materials of carbon dioxide adsorption.The specific surface area that carbon nano-fiber has is big, porosity advantages of higher gives should
Adsorbance that adsorbing material is higher and the rate of adsorption.The addition of aminated carbon nano tube can effectively promote carbon nano-fiber materials pair
The adsorptive selectivity of carbon dioxide and the mechanical property of material itself, therefore can overcome granular materials because of its structure discontinuity
The applied defect brought with easy efflorescence, can meet the needs of carbon dioxide in flue gas trapping.The carbon that the present invention is obtained is received
Rice fiber adsorbing material has preferable adsorption capacity, higher selectivity and cyclical stability to carbon dioxide, prepared
Carbon nano-fiber has good flexibility and mechanical strength, workable, and the carbon dioxide that can meet different discharge place is caught
Collection needs.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Within the scope of.
Aminated carbon nano tube in following embodiment is commercially available prod, external diameter 8～15nm, internal diameter 2～4nm, length
0.5～55 μm, specific surface area ＞ 233m2/g。
Room temperature in the present invention refers to 25 DEG C.
In embodiment 1～10, the aminated carbon nano tube purity of doping is more than 95%, and amine groups content is 0.45wt%, compares table
Area is more than 233m2/g；Spinning polymer select polyacrylonitrile (molecular weight is 12W), polyimides (molecular weight be 2W～
5W), polyvinyl butyral resin (molecular weight is 17～25W), polyaniline (molecular weight is 12W), polypyrrole (molecular weight be 17～
25W), polybenzimidazoles (molecular weight is 17～25W), phenolic resin (molecular weight is 13W), polyvinylpyrrolidone (molecular weight
Be 20～25W), polyvinyl alcohol (molecular weight is 11～13W)；Solvent select DMF, N-Methyl pyrrolidone,
Chloroform, N,N-dimethylacetamide, methanol, ethanol, deionized water, produced by Shanghai crystalline substance pure reagent company limited；High-tension electricity
The DW-P303-1ACD8 type that selection Tianjin, source Dong Wen high voltage power supply factory produces.
Embodiment 1
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.05g aminated carbon nano tube in 9.45gN, dinethylformamide with
Supersonic frequency is that 20kHz carries out ultrasonic disperse 1h, is then added in above-mentioned dispersion liquid by 0.5g polyacrylonitrile and stirs to completely
Dissolving, obtain the electrospinning raw material that mass fraction is 5%, wherein, the mass fraction of aminated carbon nano tube is 0.5%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 10kV at electrostatic pressure, syringe pump flow velocity is
0.3mL/h, spinning head is away from receiving screen distance for carrying out electrostatic spinning under conditions of 6cm, obtain containing aminated carbon nano tube is miscellaneous
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first at sky
It is warming up to 150 DEG C under gas atmosphere and carries out pre-oxidation treatment 0.5h, be warming up to 800 DEG C the most under nitrogen protection, carry out at carbonization
Reason 2h, is subsequently reduced to room temperature, it is thus achieved that the carbon nano-fiber adsorbing material of aminated carbon nano tube doping.
Embodiment 2
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.05g aminated carbon nano tube in 9.25gN, dinethylformamide with
Supersonic frequency is that 20kHz carries out ultrasonic disperse 2h, is then added in above-mentioned dispersion liquid by 0.7g polyimides and stirs to completely
Dissolving, obtain the electrospinning raw material that mass fraction is 7%, wherein, the mass fraction of aminated carbon nano tube is 0.5%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 15kV at electrostatic pressure, syringe pump flow velocity is
0.5mL/h, spinning head is away from receiving screen distance for carrying out electrostatic spinning under conditions of 10cm, obtain containing aminated carbon nano tube is miscellaneous
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first at sky
It is warming up to 180 DEG C under gas atmosphere and carries out pre-oxidation treatment 1.4h, under helium is protected, be warming up to 850 DEG C afterwards, carry out at carbonization
Reason 4h, is subsequently reduced to room temperature, it is thus achieved that the carbon nano-fiber adsorbing material of aminated carbon nano tube doping.
Embodiment 3
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.1g aminated carbon nano tube in 8.9gN, dinethylformamide with super
Acoustic frequency is that 21kHz carries out ultrasonic disperse 3h, then 1g polyvinyl butyral resin adds stirring in above-mentioned dispersion liquid the completeest to
CL, obtains the electrospinning raw material that mass fraction is 10%, and wherein, the mass fraction of aminated carbon nano tube is 1%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 20kV at electrostatic pressure, syringe pump flow velocity is
1mL/h, spinning head for carrying out electrostatic spinning under conditions of 15cm, obtains the hydridization containing aminated carbon nano tube away from receiving screen distance
Nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 200 DEG C in air atmosphere and carries out pre-oxidation treatment 2h, afterwards
It is warming up to 900 DEG C under nitrogen protection, carries out carbonization treatment 5h, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube doping
Carbon nano-fiber adsorbing material.
Embodiment 4
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.1g aminated carbon nano tube in 8.9g N-Methyl pyrrolidone with ultrasonic
Frequency is that 21kHz carries out ultrasonic disperse 5h, is then added in above-mentioned dispersion liquid by 1g polyaniline and stirs to being completely dissolved, obtains
Mass fraction is the electrospinning raw material of 10%, and wherein, the mass fraction of aminated carbon nano tube is 1%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 15kV at electrostatic pressure, syringe pump flow velocity is
1mL/h, spinning head for carrying out electrostatic spinning under conditions of 15cm, obtains the hydridization containing aminated carbon nano tube away from receiving screen distance
Nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 200 DEG C in air atmosphere and carries out pre-oxidation treatment 2h, afterwards
Under argon shield, it is warming up to 900 DEG C, carries out 8h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube doping
Carbon nano-fiber adsorbing material.
Embodiment 5
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.1g aminated carbon nano tube in 8.7g chloroform with supersonic frequency as 22kHz
Carry out ultrasonic disperse 6h, then 1.2g polypyrrole is added in above-mentioned dispersion liquid and stir to being completely dissolved, obtain mass fraction
Being the electrospinning raw material of 12%, wherein, the mass fraction of aminated carbon nano tube is 1%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 20kV at electrostatic pressure, syringe pump flow velocity is
1.5mL/h, spinning head is away from receiving screen distance for carrying out electrostatic spinning under conditions of 15cm, obtain containing aminated carbon nano tube is miscellaneous
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 220 DEG C in air atmosphere and carries out pre-oxidation treatment 2.6h, it
After xenon protect under be warming up to 900 DEG C, carry out 10h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube adulterate
Carbon nano-fiber adsorbing material.
Embodiment 6
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.1g aminated carbon nano tube in 8.4g N,N-dimethylacetamide with super
Acoustic frequency is that 22kHz carries out ultrasonic disperse 7h, is then added in above-mentioned dispersion liquid by 1.5g polybenzimidazoles and stirs to completely
Dissolving, obtain the electrospinning raw material that mass fraction is 15%, wherein, the mass fraction of aminated carbon nano tube is 1%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 25kV at electrostatic pressure, syringe pump flow velocity is
2mL/h, spinning head for carrying out electrostatic spinning under conditions of 15cm, obtains the hydridization containing aminated carbon nano tube away from receiving screen distance
Nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 250 DEG C in air atmosphere and carries out pre-oxidation treatment 3.5h, it
After be warming up to 950 DEG C under nitrogen protection, carry out 12h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube adulterate
Carbon nano-fiber adsorbing material.
Embodiment 7
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.15g aminated carbon nano tube in 7.85g methanol with supersonic frequency it is
23kHz carries out ultrasonic disperse 8h, is then added in above-mentioned dispersion liquid by 2g phenolic resin and stirs to being completely dissolved, obtains quality
Mark is the electrospinning raw material of 20%, and wherein, the mass fraction of aminated carbon nano tube is 1.5%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 30kV at electrostatic pressure, syringe pump flow velocity is
2.5mL/h, spinning head is away from receiving screen distance for carrying out electrostatic spinning under conditions of 15cm, obtain containing aminated carbon nano tube is miscellaneous
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 260 DEG C in air atmosphere and carries out pre-oxidation treatment 3.8h, it
After be warming up to 1000 DEG C under nitrogen protection, carry out 15h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube is mixed
Miscellaneous carbon nano-fiber adsorbing material.
Embodiment 8
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.15g aminated carbon nano tube in 7.35g ethanol with supersonic frequency it is
23kHz carries out ultrasonic disperse 8h, is then added to by 2.5g polyvinylpyrrolidone and stirs in above-mentioned dispersion liquid to being completely dissolved,
Obtaining the electrospinning raw material that mass fraction is 25%, wherein, the mass fraction of aminated carbon nano tube is 1.5%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 30kV at electrostatic pressure, syringe pump flow velocity is
3mL/h, spinning head for carrying out electrostatic spinning under conditions of 20cm, obtains the hydridization containing aminated carbon nano tube away from receiving screen distance
Nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 280 DEG C in air atmosphere and carries out pre-oxidation treatment 4.4h, it
After xenon protect under be warming up to 1200 DEG C, carry out 16h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube is mixed
Miscellaneous carbon nano-fiber adsorbing material.
Embodiment 9
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first 0.4g aminated carbon nano tube is entered with supersonic frequency for 24kHz in 7.1g water
Row ultrasonic disperse 9h, then adds to 2.5g polyvinyl alcohol in above-mentioned dispersion liquid and stirs to being completely dissolved, obtain mass fraction
Being the electrospinning raw material of 25%, wherein, the mass fraction of aminated carbon nano tube is 4%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 35kV at electrostatic pressure, syringe pump flow velocity is
3.5mL/h, spinning head is away from receiving screen distance for carrying out electrostatic spinning under conditions of 20cm, obtain containing aminated carbon nano tube is miscellaneous
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 300 DEG C in air atmosphere and carries out pre-oxidation treatment 5h, afterwards
It is warming up to 1400 DEG C under nitrogen protection, carries out 18h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube adulterates
Carbon nano-fiber adsorbing material.
Embodiment 10
The preparation method of the carbon nano-fiber adsorbing material of a kind of aminated carbon nano tube doping, concretely comprises the following steps:
(1) at room temperature 25 DEG C, first by 0.5g aminated carbon nano tube in 6.5g DMF with super
Acoustic frequency is that 25kHz carries out ultrasonic disperse 10h, is then added in above-mentioned dispersion liquid by 3g ethyl cellulose and stirs to the most molten
Solving, obtain the electrospinning raw material that mass fraction is 30%, wherein, the mass fraction of aminated carbon nano tube is 5%；
(2) joining in electrostatic spinning apparatus by the electrospinning raw material obtained, be 40kV at electrostatic pressure, syringe pump flow velocity is
4mL/h, spinning head for carrying out electrostatic spinning under conditions of 20cm, obtains the hydridization containing aminated carbon nano tube away from receiving screen distance
Nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is carried out carbonization treatment, concretely comprise the following steps: first will contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 300 DEG C in air atmosphere and carries out pre-oxidation treatment 5h, afterwards
It is warming up to 1600 DEG C under nitrogen protection, carries out 20h carbonization treatment, be subsequently reduced to room temperature, it is thus achieved that aminated carbon nano tube adulterates
Carbon nano-fiber adsorbing material.
Embodiment 11
The carbon nano-fiber adsorbing material adulterating the aminated carbon nano tube of above-mentioned preparation is evaluated:
1, synchronization thermogravimetric analyzer (TA-Q600TGA/DSC) is utilized to measure the amination prepared by embodiment 1～10 respectively
Carbon nano tube-doped carbon nano-fiber adsorbing material CO at 40 DEG C2Adsorbance.Experimental result see table:
Conclusion: as can be seen from the above table, the aminated carbon nano tube prepared according to the method described in embodiment 1～10
The carbon nano-fiber adsorbing material of doping is to CO2Adsorbance increase with the increase of aminated carbon nano tube mass fraction, its
To CO2Adsorbance be superior to the absorption property of commercial activated carbon, maximum can reach the adsorbance of 7.5mmol/g.Therefore basis
The carbon nano-fiber adsorbing material of aminated carbon nano tube doping prepared by embodiment of the present invention method has good CO2Absorption
Performance.
2, the carbon nano-fiber adsorbing material adulterating the aminated carbon nano tube of above-mentioned preparation is to CO2Relative to N2Suction
Attached selective evaluation.
Experimental technique: the carbon nano-fiber adsorbing material that the aminated carbon nano tube prepared by embodiment 1～10 is adulterated
It is placed in CO2In atmosphere, at 25 DEG C, change CO2Pressure；In like manner, this material is placed in N2In atmosphere, at 25 DEG C, change N2's
Pressure.At 25 DEG C, adsorbing material is for CO2Selectivity tried to achieve by below equation: S (CO2/N2)=(q1/q2)/(x1/x2), its
Middle q1For CO2Adsorbance under 0.15bar, q2For N2Adsorbance under 0.75bar, x1For CO2Dividing potential drop 0.15bar, x2
For N2Dividing potential drop 0.75bar.Experimental result see table:
Conclusion: as can be seen from the above table, the carbon nanometer adulterated according to the aminated carbon nano tube prepared by embodiment 1～10
Fiber adsorbing material is to CO2Relative to N2Selectivity be 25～72, and S with aminated carbon nano tube mass fraction increase and
Increase.Illustrate prepared by the present invention aminated carbon nano tube doping carbon nano-fiber adsorbing material to flue gas (smoke components:
CO215%, N275%) CO in2There is fabulous adsorption selectivity.
Claims (8)
1. the preparation method of the carbon nano-fiber adsorbing material of an aminated carbon nano tube doping, it is characterised in that including:
The first step: at room temperature, first by aminated carbon nano tube ultrasonic disperse 1～10h in a solvent, then by carbon Nanowire
The precursor polymer of dimension is added in above-mentioned dispersion liquid and is stirred to being completely dissolved, and obtains the electrospinning that mass fraction is 5～30%
Raw material；
Second step: the electrospinning raw material first step obtained joins in electrostatic spinning apparatus, carries out electrostatic spinning, obtains containing amino
The Hybrid nanofibers material of carbon nano tube；
3rd step: the Hybrid nanofibers material containing aminated carbon nano tube prepared by second step carries out carbonization treatment, it is thus achieved that
The carbon nano-fiber adsorbing material of aminated carbon nano tube doping.
2. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 1, it is special
Levying and be, described electrospinning conditions is: electrostatic pressure is 10-40kV, and syringe pump flow velocity is 0.3～4mL/h, and spinning head is away from connecing
Receiving screen distance is 6～20cm.
3. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 1, it is special
Levying and be, described aminated carbon nano tube is amination multi-walled carbon nano-tubes, external diameter 8～15nm, internal diameter 2～4nm, length
0.5～55 μm, specific surface area ＞ 233m2/ g, aminated carbon nano tube mass fraction in electrospinning raw material is 0.5～5%.
4. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 1, it is special
Levying and be, described solvent is DMF, Methanamide, oxolane, N-Methyl pyrrolidone, chloroform, N, N-
Dimethyl acetylamide, methanol, ethanol, water, acetone, dichloromethane, formic acid, acetic acid, dimethyl sulfoxide, ether, trichloroacetic acid, three
One or more mixture in Fluoroethanoic acid and pyridine.
5. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 1, it is special
Levying and be, described precursor polymer is polyacrylonitrile, polyimides, polyvinyl butyral resin, polybenzoxazine, polyphenyl
Amine, polypyrrole, polybenzimidazoles, phenolic resin, polyvinylpyrrolidone, polyvinyl alcohol, cellulose, cellulose acetate and second
One or more mixture in base cellulose.
6. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 1, it is special
Levying and be, described carbonization treatment includes: be first warming up in air atmosphere 150～300 DEG C carry out pre-oxidation treatment 0.5～
5h, is warming up to 600～1600 DEG C afterwards under inert gas shielding, carries out carbonization treatment 0.5～20h, lowers the temperature subsequently.
7. the preparation method of the carbon nano-fiber adsorbing material of aminated carbon nano tube doping as claimed in claim 6, it is special
Levying and be, described protective gas is the combination of one or more in nitrogen, helium, neon, argon, Krypton, xenon.
8. the preparation of the carbon nano-fiber adsorbing material of the aminated carbon nano tube doping according to any one of claim 1～7
The carbon nano-fiber adsorbing material of the aminated carbon nano tube doping prepared by method.
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