CN106268636B - The carbon nano-fiber adsorbent material and preparation method thereof of aminated carbon nano tube doping - Google Patents
The carbon nano-fiber adsorbent material and preparation method thereof of aminated carbon nano tube doping Download PDFInfo
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- CN106268636B CN106268636B CN201610664022.7A CN201610664022A CN106268636B CN 106268636 B CN106268636 B CN 106268636B CN 201610664022 A CN201610664022 A CN 201610664022A CN 106268636 B CN106268636 B CN 106268636B
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- nano tube
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000000463 material Substances 0.000 title claims abstract description 89
- 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
- 239000003463 adsorbent Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 238000011282 treatment Methods 0.000 claims abstract description 36
- 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
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 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
- 238000009987 spinning Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 12
- 239000007924 injection Substances 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000000034 method Methods 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
- 239000007789 gas Substances 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 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
- 239000000203 mixture Substances 0.000 claims description 5
- 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
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-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
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 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
- 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
- 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
- 125000002924 primary amino group Chemical group [H]N([H])* 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
- 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
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- QEWYKACRFQMRMB-UHFFFAOYSA-N fluoroacetic acid Chemical compound OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims 2
- 239000011261 inert gas Substances 0.000 claims 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
- -1 polybenzoxazine Polymers 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 29
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 23
- 229960004424 carbon dioxide Drugs 0.000 abstract description 15
- 239000001569 carbon dioxide Substances 0.000 abstract description 13
- 238000001179 sorption measurement Methods 0.000 abstract description 12
- 235000011089 carbon dioxide Nutrition 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 description 8
- 239000003575 carbonaceous material Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000010410 dusting Methods 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000000835 fiber 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
- 229920002873 Polyethylenimine Polymers 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
- 239000008187 granular material Substances 0.000 description 2
- 230000001681 protective effect Effects 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
- 238000005576 amination reaction Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 239000013065 commercial product 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
- 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
- 238000004519 manufacturing process 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
- 239000002245 particle Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 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
- 239000000243 solution Substances 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 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)
- Nonwoven Fabrics (AREA)
- Artificial Filaments (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of preparation methods of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, it is characterized in that, it include: step 1: at room temperature, first by aminated carbon nano tube 1~10h of ultrasonic disperse in a solvent, then the precursor polymer of carbon nano-fiber is added to stir in above-mentioned dispersion liquid and obtains the electrospinning raw material that mass fraction is 5~30% to being completely dissolved；Step 2: the electrospinning raw material that the first step obtains is added in electrostatic spinning apparatus, electrostatic spinning is carried out, the Hybrid nanofibers material containing aminated carbon nano tube is obtained；Step 3: the Hybrid nanofibers material containing aminated carbon nano tube of second step preparation is carried out carbonization treatment, the carbon nano-fiber adsorbent material of aminated carbon nano tube doping is obtained.Present invention carbon nano-fiber adsorbent material obtained has preferable adsorption capacity, higher selectivity and cyclical stability to carbon dioxide, can meet the collecting carbonic anhydride needs in different discharge places.
Description
Technical field
The present invention relates to a kind of carbon nano-fiber adsorbent materials and preparation method thereof of aminated carbon nano tube doping, belong to
Carbon dioxide adsorption technical field.
Background technique
A large amount of use of fossil fuel causes the gas concentration lwevel in atmosphere to increase year by year, greenhouse effects is caused to highlight,
A series of environment frequently occur etc. for the rising of earth surface temperature, Melting Glacierss, sea-level rise, Extreme Weather Events and ecology is asked
Topic, therefore the trapping and storage of carbon dioxide are extremely important.Absorption method is due to, selectivity big with adsorption capacity
It is high, low energy consumption and it is easily separated the advantages that and receive significant attention, become collecting carbonic anhydride and field of storage research hotspot it
One.Porous active Carbon Materials have many advantages, such as that specific surface area is high, pore structure is abundant, chemical property and macroscopic property are stablized, and are
Solid absorbent is used in a kind of common carbon dioxide adsorption separation.But pure carbon material is mainly object to the suction-operated of carbon dioxide
Reason absorption causes its carbon dioxide adsorption and selectivity all poor.Being modified using amine substance to carbon material can be improved
The carbon dioxide adsorption selectivity of material, " a kind of two based on ordered mesopore carbon as disclosed in domestic patent CN105289530A
Aoxidize carbon adsorbent and preparation method ", which is to load to polyethyleneimine on carbon material by infusion process to improve suction
Attached selectivity, but the load of polyethyleneimine significantly reduces the specific surface area and porosity of carbon material.In addition, existing particle
Shape carbon material in use generally existing easy dusting the problem of, limit its operability and practical application performance.Carbon is received
The structural advantages such as rice fibrous material is good with its continuity, cellular structure is abundant, can effectively overcome granular materials not connect because of its structure
Applied defect brought by continuous property and easy dusting, shows huge application potential in adsorbing separation field, but how to improve
The carbon dioxide adsorption selectivity and mechanical performance of carbon nano-fiber are still a problem urgently to be resolved.
Summary of the invention
The object of the present invention is to provide a kind of preparation sides of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping
Method, to solve the problems, such as carbon nano-fiber adsorptive selectivity difference and carbon material generally existing easy dusting in use.
In order to achieve the above object, the present invention provides a kind of carbon nano-fiber adsorption materials of aminated carbon nano tube doping
The preparation method of material characterized by comprising
Step 1: at room temperature, first by aminated carbon nano tube 1~10h of ultrasonic disperse in a solvent, then carbon is received
The precursor polymer of rice fiber, which is added in above-mentioned dispersion liquid, to be stirred to being completely dissolved, and obtaining mass fraction is 5~30%
Electrospinning raw material；
Step 2: the electrospinning raw material that the first step obtains is added in electrostatic spinning apparatus, electrostatic spinning is carried out, is contained
The Hybrid nanofibers material of aminated carbon nano tube；
Step 3: the Hybrid nanofibers material containing aminated carbon nano tube of second step preparation is subjected to carbonization treatment,
Obtain the carbon nano-fiber adsorbent material of aminated carbon nano tube doping.
Preferably, the electrospinning conditions are as follows: electrostatic pressure is 10~40kV, and injection flow rate pump 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 first step uses is 20~25kHz.
Preferably, the aminated carbon nano tube be amino multi-wall carbon nanotube, 8~15nm of outer diameter, internal diameter 2~
4nm, 0.5~55 μm of length, specific surface area > 233m2/ g, mass fraction of the aminated carbon nano tube in electrospinning raw material are 0.5
~5%.
Preferably, the solvent is the solvent for dissolving precursor polymer.
It is highly preferred that the solvent be n,N-Dimethylformamide, formamide, tetrahydrofuran, N-Methyl pyrrolidone,
Chloroform, n,N-dimethylacetamide, methanol, ethyl alcohol, water, acetone, methylene chloride, formic acid, acetic acid, dimethyl sulfoxide, ether, three
The mixture of one or more of monoxone, trifluoroacetic acid and pyridine.
Preferably, the precursor polymer is polyacrylonitrile, polyimides, polyvinyl butyral, polyphenyl and dislikes
Piperazine, polyaniline, polypyrrole, polybenzimidazoles, phenolic resin, polyvinylpyrrolidone, polyvinyl alcohol, cellulose, acetate fiber
The mixture of one or more of plain and ethyl cellulose.
Preferably, the carbonization treatment includes: and is first warming up to 150~300 DEG C in air atmosphere to carry out at pre-oxidation
0.5~5h is managed, is warming up to 600~1600 DEG C under protective gas protection later, 0.5~20h of carbonization treatment is carried out, then drops
Temperature.
It is highly preferred that the protective gas is one of nitrogen, helium, neon, argon gas, Krypton, xenon or a variety of
Combination.
The present invention also provides the carbon nano-fiber adsorbent materials of the aminated carbon nano tube doping prepared by the above method.
Advantages of the present invention is as follows compared with prior art:
Present invention process is simple, by adulterating aminated carbon nano tube in carbon nano-fiber surface and interface, can be used for
The carbon nano-fiber materials of carbon dioxide adsorption.Large specific surface area that carbon nano-fiber has, the advantages that porosity is high assign should
The higher adsorbance of adsorbent material 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 granular materials can be overcome because of its structure discontinuity
With applied defect brought by easy dusting, the needs of carbon dioxide in flue gas trapping can be met.Present invention carbon 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 flexible and mechanical strength, strong operability, and the carbon dioxide that can meet different discharge places is caught
Collection needs.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Within the scope of.
Aminated carbon nano tube in following embodiment is commercial product, 8~15nm of outer diameter, 2~4nm of internal diameter, length
0.5~55 μm, specific surface area > 233m2/g。
Room temperature in the present invention refers to 25 DEG C.
The aminated carbon nano tube purity adulterated in Examples 1 to 10 is greater than 95%, and amine groups content 0.45wt% compares table
Area is greater than 233m2/g；Spinning with polymer select polyacrylonitrile (molecular weight 12W), polyimides (molecular weight be 2W~
5W), polyvinyl butyral (molecular weight is 17~25W), polyaniline (molecular weight 12W), polypyrrole (molecular weight is 17~
25W), polybenzimidazoles (molecular weight is 17~25W), phenolic resin (molecular weight 13W), polyvinylpyrrolidone (molecular weight
For 20~25W), polyvinyl alcohol (molecular weight is 11~13W)；Solvent select n,N-Dimethylformamide, N-Methyl pyrrolidone,
Chloroform, n,N-dimethylacetamide, methanol, ethyl alcohol, deionized water are produced by Shanghai crystalline substance pure reagent Co., Ltd；High-voltage electricity
The DW-P303-1ACD8 type of Tianjin Dong Wen high voltage power supply factory production is selected in source.
Embodiment 1
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.05g aminated carbon nano tube in 9.45gN, dinethylformamide with
Supersonic frequency is that 20kHz carries out ultrasonic disperse 1h, and then 0.5g polyacrylonitrile is added in above-mentioned dispersion liquid and stirs to complete
Dissolution obtains the electrospinning raw material that mass fraction is 5%, wherein the mass fraction of aminated carbon nano tube is 0.5%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 10kV in electrostatic pressure, injection flow rate pump is
0.3mL/h, spinning head, to carry out electrostatic spinning under conditions of 6cm, are obtained containing the miscellaneous of aminated carbon nano tube away from receiving screen distance
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is subjected to carbonization treatment, specific steps are as follows: first in sky
It is warming up to 150 DEG C of progress pre-oxidation treatment 0.5h under gas atmosphere, is warming up to 800 DEG C under nitrogen protection later, carries out at carbonization
2h is managed, room temperature is subsequently reduced to, obtains the carbon nano-fiber adsorbent material of aminated carbon nano tube doping.
Embodiment 2
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.05g aminated carbon nano tube in 9.25gN, dinethylformamide with
Supersonic frequency is that 20kHz carries out ultrasonic disperse 2h, and then 0.7g polyimides is added in above-mentioned dispersion liquid and stirs to complete
Dissolution obtains the electrospinning raw material that mass fraction is 7%, wherein the mass fraction of aminated carbon nano tube is 0.5%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 15kV in electrostatic pressure, injection flow rate pump is
0.5mL/h, spinning head, to carry out electrostatic spinning under conditions of 10cm, are obtained containing the miscellaneous of aminated carbon nano tube away from receiving screen distance
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is subjected to carbonization treatment, specific steps are as follows: first in sky
It is warming up to 180 DEG C of progress pre-oxidation treatment 1.4h under gas atmosphere, is warming up to 850 DEG C under helium protection later, carries out at carbonization
4h is managed, room temperature is subsequently reduced to, obtains the carbon nano-fiber adsorbent material of aminated carbon nano tube doping.
Embodiment 3
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.1g aminated carbon nano tube in 8.9gN, dinethylformamide with super
Acoustic frequency is that 21kHz carries out ultrasonic disperse 3h, and then 1g polyvinyl butyral is added in above-mentioned dispersion liquid and stirs to complete
Fully dissolved obtains the electrospinning raw material that mass fraction is 10%, wherein the mass fraction of aminated carbon nano tube is 1%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 20kV in electrostatic pressure, injection flow rate pump is
1mL/h, spinning head, to carry out electrostatic spinning under conditions of 15cm, obtain 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 subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 200 DEG C of progress pre-oxidation treatment 2h in air atmosphere, later
It is warming up to 900 DEG C under nitrogen protection, carries out carbonization treatment 5h, is subsequently reduced to room temperature, obtains aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 4
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.1g aminated carbon nano tube in 8.9g N-Methyl pyrrolidone with ultrasound
Frequency is that 21kHz carries out ultrasonic disperse 5h, and then 1g polyaniline is added in above-mentioned dispersion liquid and stirs to being completely dissolved, obtains
The electrospinning raw material that mass fraction is 10%, wherein the mass fraction of aminated carbon nano tube is 1%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 15kV in electrostatic pressure, injection flow rate pump is
1mL/h, spinning head, to carry out electrostatic spinning under conditions of 15cm, obtain 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 subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 200 DEG C of progress pre-oxidation treatment 2h in air atmosphere, later
It is warming up to 900 DEG C under protection of argon gas, carries out 8h carbonization treatment, is subsequently reduced to room temperature, obtains aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 5
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
It (1) with supersonic frequency is first 22kHz in 8.7g chloroform by 0.1g aminated carbon nano tube at 25 DEG C of room temperature
Ultrasonic disperse 6h is carried out, then 1.2g polypyrrole is added in above-mentioned dispersion liquid and stirs to being completely dissolved, obtains mass fraction
For 12% electrospinning raw material, wherein the mass fraction of aminated carbon nano tube is 1%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 20kV in electrostatic pressure, injection flow rate pump is
1.5mL/h, spinning head, to carry out electrostatic spinning under conditions of 15cm, are obtained containing the miscellaneous of aminated carbon nano tube away from receiving screen distance
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 220 DEG C of progress pre-oxidation treatment 2.6h in air atmosphere, it
900 DEG C are warming up under xenon protection afterwards, carries out 10h carbonization treatment, is subsequently reduced to room temperature, obtains aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 6
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, 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, and then 1.5g polybenzimidazoles is added in above-mentioned dispersion liquid and stirs to complete
Dissolution obtains the electrospinning raw material that mass fraction is 15%, wherein the mass fraction of aminated carbon nano tube is 1%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 25kV in electrostatic pressure, injection flow rate pump is
2mL/h, spinning head, to carry out electrostatic spinning under conditions of 15cm, obtain 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 subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 250 DEG C of progress pre-oxidation treatment 3.5h in air atmosphere, it
It is warming up to 950 DEG C under nitrogen protection afterwards, carries out 12h carbonization treatment, be subsequently reduced to room temperature, obtain aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 7
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, it is with supersonic frequency in 7.85g methanol by 0.15g aminated carbon nano tube first
23kHz carries out ultrasonic disperse 8h, and then 2g phenolic resin is added in above-mentioned dispersion liquid and stirs to being completely dissolved, obtains quality
The electrospinning raw material that score is 20%, wherein the mass fraction of aminated carbon nano tube is 1.5%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 30kV in electrostatic pressure, injection flow rate pump is
2.5mL/h, spinning head, to carry out electrostatic spinning under conditions of 15cm, are obtained containing the miscellaneous of aminated carbon nano tube away from receiving screen distance
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 260 DEG C of progress pre-oxidation treatment 3.8h in air atmosphere, it
It is warming up to 1000 DEG C under nitrogen protection afterwards, carries out 15h carbonization treatment, be subsequently reduced to room temperature, obtain aminated carbon nano tube and mix
Miscellaneous carbon nano-fiber adsorbent material.
Embodiment 8
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, it is with supersonic frequency in 7.35g ethyl alcohol by 0.15g aminated carbon nano tube first
23kHz carries out ultrasonic disperse 8h, and then 2.5g polyvinylpyrrolidone is added in above-mentioned dispersion liquid and stirs to being completely dissolved,
Obtain the electrospinning raw material that mass fraction is 25%, wherein the mass fraction of aminated carbon nano tube is 1.5%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 30kV in electrostatic pressure, injection flow rate pump is
3mL/h, spinning head, to carry out electrostatic spinning under conditions of 20cm, obtain 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 subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 280 DEG C of progress pre-oxidation treatment 4.4h in air atmosphere, it
1200 DEG C are warming up under xenon protection afterwards, carries out 16h carbonization treatment, is subsequently reduced to room temperature, aminated carbon nano tube is obtained and mixes
Miscellaneous carbon nano-fiber adsorbent material.
Embodiment 9
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.4g aminated carbon nano tube in 7.1g water with supersonic frequency be 24kHz into
2.5g polyvinyl alcohol, is then added in above-mentioned dispersion liquid and stirs to being completely dissolved, obtain mass fraction by row ultrasonic disperse 9h
For 25% electrospinning raw material, wherein the mass fraction of aminated carbon nano tube is 4%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 35kV in electrostatic pressure, injection flow rate pump is
3.5mL/h, spinning head, to carry out electrostatic spinning under conditions of 20cm, are obtained containing the miscellaneous of aminated carbon nano tube away from receiving screen distance
Change nano-fiber material；
(3) the Hybrid nanofibers material containing aminated carbon nano tube is subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 300 DEG C of progress pre-oxidation treatment 5h in air atmosphere, later
It is warming up to 1400 DEG C under nitrogen protection, carries out 18h carbonization treatment, is subsequently reduced to room temperature, obtains aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 10
A kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping, specific steps are as follows:
(1) at 25 DEG C of room temperature, first by 0.5g aminated carbon nano tube in 6.5g n,N-Dimethylformamide with super
Acoustic frequency is that 25kHz carries out ultrasonic disperse 10h, and then 3g ethyl cellulose is added in above-mentioned dispersion liquid and stirs to completely molten
Solution obtains the electrospinning raw material that mass fraction is 30%, wherein the mass fraction of aminated carbon nano tube is 5%；
(2) obtained electrospinning raw material is added in electrostatic spinning apparatus, is 40kV in electrostatic pressure, injection flow rate pump is
4mL/h, spinning head, to carry out electrostatic spinning under conditions of 20cm, obtain 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 subjected to carbonization treatment, specific steps are as follows: will first contain
The Hybrid nanofibers material of aminated carbon nano tube is warming up to 300 DEG C of progress pre-oxidation treatment 5h in air atmosphere, later
It is warming up to 1600 DEG C under nitrogen protection, carries out 20h carbonization treatment, is subsequently reduced to room temperature, obtains aminated carbon nano tube doping
Carbon nano-fiber adsorbent material.
Embodiment 11
The carbon nano-fiber adsorbent material of the aminated carbon nano tube doping of above-mentioned preparation is evaluated:
1, amination prepared by Examples 1 to 10 is measured respectively using synchronous thermogravimetric analyzer (TA-Q600TGA/DSC)
CO of the carbon nano tube-doped carbon nano-fiber adsorbent material at 40 DEG C2Adsorbance.Experimental result see the table below:
Conclusion: as can be seen from the above table, the aminated carbon nano tube that the method according to Examples 1 to 10 is prepared
The carbon nano-fiber adsorbent material of doping is to CO2Adsorbance increase with the increase of aminated carbon nano tube mass fraction,
To CO2Adsorbance be superior to the absorption property of commercial active carbon, maximum can reach the adsorbance of 7.5mmol/g.Therefore basis
The carbon nano-fiber adsorbent material of the aminated carbon nano tube doping of present invention method preparation has good CO2Absorption
Performance.
2, to the carbon nano-fiber adsorbent material of the aminated carbon nano tube doping of above-mentioned preparation to CO2Relative to N2Suction
Attached selective evaluation.
Experimental method: the carbon nano-fiber adsorbent material that aminated carbon nano tube prepared by Examples 1 to 10 is adulterated
It is placed in CO2In atmosphere, change CO at 25 DEG C2Pressure；Similarly, which is placed in N2In atmosphere, change N at 25 DEG C2's
Pressure.Adsorbent material is for CO at 25 DEG C2Selectivity acquired by following formula: S (CO2/N2)=(q1/q2)/(x1/x2),
Middle q1For CO2Adsorbance at 0.15bar, q2For N2Adsorbance at 0.75bar, x1For CO2Partial pressure 0.15bar, x2
For N2Partial pressure 0.75bar.Experimental result see the table below:
Conclusion: as can be seen from the above table, the carbon nanometer of the doping of the aminated carbon nano tube according to prepared by Examples 1 to 10
Fiber adsorbing material is to CO2Relative to N2Selectivity be 25~72, and S with the increase of aminated carbon nano tube mass fraction and
Increase.Illustrate aminated carbon nano tube prepared by the present invention doping carbon nano-fiber adsorbent material to flue gas (smoke components:
CO215%, N275%) CO in2With fabulous adsorption selectivity.
Claims (7)
1. a kind of preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping characterized by comprising
Step 1: at room temperature, first by aminated carbon nano tube 1~10h of ultrasonic disperse in a solvent, supersonic frequency is 20~
Then the precursor polymer of carbon nano-fiber is added in above-mentioned dispersion liquid and stirs to being completely dissolved, obtains quality by 25kHz
The electrospinning raw material that score is 5~30%；The aminated carbon nano tube be amino multi-wall carbon nanotube, 8~15nm of outer diameter,
2~4nm of internal diameter, 0.5~55 μm of length, specific surface area > 233m2/ g, quality of the aminated carbon nano tube in electrospinning raw material point
Number is 0.5~5%；
Step 2: the electrospinning raw material that the first step obtains is added in electrostatic spinning apparatus, electrostatic spinning is carried out, is obtained containing amino
The Hybrid nanofibers material of carbon nano tube；
Step 3: the Hybrid nanofibers material containing aminated carbon nano tube of second step preparation is carried out carbonization treatment, obtain
The carbon nano-fiber adsorbent material of aminated carbon nano tube doping.
2. the preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping as described in claim 1, special
Sign is, the electrospinning conditions are as follows: electrostatic pressure 10-40kV, injection flow rate pump are 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 adsorbent material of aminated carbon nano tube doping as described in claim 1, special
Sign is that the solvent is n,N-Dimethylformamide, formamide, tetrahydrofuran, N-Methyl pyrrolidone, chloroform, N, N-
Dimethyl acetamide, methanol, ethyl alcohol, water, acetone, methylene chloride, formic acid, acetic acid, dimethyl sulfoxide, ether, trichloroacetic acid, three
The mixture of one or more of fluoroacetic acid and pyridine.
4. the preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping as described in claim 1, special
Sign is that the precursor polymer is polyacrylonitrile, polyimides, polyvinyl butyral, polybenzoxazine, polyphenyl
Amine, polypyrrole, polybenzimidazoles, phenolic resin, polyvinylpyrrolidone, polyvinyl alcohol, cellulose, cellulose acetate and second
The mixture of one or more of base cellulose.
5. the preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping as described in claim 1, special
Sign is, the carbonization treatment include: first be warming up in air atmosphere 150~300 DEG C of progress pre-oxidation treatments 0.5~
5h is warming up to 600~1600 DEG C under inert gas or nitrogen protection later, carries out 0.5~20h of carbonization treatment, then cools down.
6. the preparation method of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping as claimed in claim 5, special
Sign is that the inert gas is one of helium, neon, argon gas, Krypton, xenon or a variety of combinations.
7. the preparation of the carbon nano-fiber adsorbent material of aminated carbon nano tube doping according to any one of claims 1 to 6
The carbon nano-fiber adsorbent material of the doping of aminated carbon nano tube prepared by method.
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| CN111266088B (en) * | 2020-01-13 | 2022-03-15 | 武汉工程大学 | Efficient porous adsorbent for treating phenolic wastewater and preparation method thereof |
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| CN113788970B (en) * | 2021-10-19 | 2022-11-22 | 江南大学 | Carbon nano tube/microcrystalline cellulose composite membrane and preparation method and application thereof |
| CN115215326B (en) * | 2022-02-23 | 2023-06-30 | 无锡东恒新能源科技有限公司 | Pre-oxidation device for purifying carbon nano tube |
| CN114927355B (en) * | 2022-04-26 | 2023-07-28 | 武夷学院 | Preparation method of flexible electrode material of carbon nanotube grafted polyaniline/cellulose nanofiber membrane |
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