CN114481365A - Activated carbon fiber and method for loading carbon nano tube - Google Patents
Activated carbon fiber and method for loading carbon nano tube Download PDFInfo
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- CN114481365A CN114481365A CN202011165492.1A CN202011165492A CN114481365A CN 114481365 A CN114481365 A CN 114481365A CN 202011165492 A CN202011165492 A CN 202011165492A CN 114481365 A CN114481365 A CN 114481365A
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- carbon fiber
- activated carbon
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 23
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 23
- 238000011068 loading method Methods 0.000 title claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 16
- 239000004917 carbon fiber Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 230000004913 activation Effects 0.000 claims abstract description 10
- 238000003763 carbonization Methods 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 150000005846 sugar alcohols Polymers 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010000 carbonizing Methods 0.000 claims description 6
- 238000005229 chemical vapour deposition Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- CDVAIHNNWWJFJW-UHFFFAOYSA-N 3,5-diethoxycarbonyl-1,4-dihydrocollidine Chemical compound CCOC(=O)C1=C(C)NC(C)=C(C(=O)OCC)C1C CDVAIHNNWWJFJW-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- -1 carbon nanotube-activated carbon fiber Chemical class 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical group OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 11
- 230000004048 modification Effects 0.000 abstract description 4
- 238000012986 modification Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 150000001721 carbon Chemical class 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- LZKLAOYSENRNKR-LNTINUHCSA-N iron;(z)-4-oxoniumylidenepent-2-en-2-olate Chemical compound [Fe].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O LZKLAOYSENRNKR-LNTINUHCSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
- D01F11/125—Carbon
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention discloses an activated carbon fiber and a method for loading a carbon nano tube, belonging to the field of materials. The material is prepared by sequentially carrying out activation, pre-oxidation and carbonization processes on fibers, and then carrying out a process of loading a precursor and carbon nanotube-activated carbon fibers on modified carbon fibers to obtain a target product. The invention adopts a novel physical and chemical activation method (irradiation-chemical method) to prepare the activated carbon fiber. The method adopts a 60 Co-gamma ray irradiation method for activation, and simultaneously combines a conventional chemical method to prepare an activated carbon fiber product, thereby realizing the purpose of surface modification of the activated carbon fiber, and loading carbon nanotubes on the surface of the activated carbon fiber while surface modification of the activated carbon fiber is carried out, thereby further optimizing the structure and performance of the activated carbon fiber.
Description
Technical Field
The invention relates to the field of materials, in particular to an activated carbon fiber and a method for loading carbon nanotubes.
Background
Activated Carbon Fiber (ACF) is a functional carbon fiber which is developed in the early 70 th century and has better adsorption performance than activated carbon. The activated carbon fiber is a mesophase formed in the fiber carbonization process and has high tensile strength and elasticity. Its precursor is polymeric fibre (polyacrylonitrile, phenolic resin, polydiethylene), cellulose and asphalt (coal tar asphalt, petroleum asphalt). The activated carbon fiber has a high specific surface area (BET) of typically 1000m2/g～2000m2(iv)/g, has unique advantages not possessed by Granular Activated Carbon (GAC) and Powdered Activated Carbon (PAC), and has good processing in form and formThe product has good performance and plasticity, and can be processed into various shapes such as felt, cloth, net, sheet, honeycomb, ripple shape and the like.
At present, the prior art has the following defects:
1) the active carbon fiber prepared by the physical method has less pore structure and generally needs a pretreatment carbonization step;
2) the chemical method for preparing the activated carbon fiber needs a large amount of activating agent, but the activating agent is generally a toxic and harmful chemical which has strong corrosivity, pollutes the environment and is easy to remain, and the production process has great harm to the environment.
3) A physical and chemical method: the method combines the characteristics of physical and chemical methods, and most products prepared by the method are used for liquid phase adsorption and are less used for gas adsorption.
4) The activated carbon fiber prepared by the catalytic activation method has the defect that part of toxic and harmful metal elements remain in the activated carbon fiber, so that the application of the activated carbon fiber to liquid phase adsorption, catalyst carriers, medical industries and the like is limited.
5) An interface activation method: however, the method is in the experimental research stage, and the technology is not mature.
Disclosure of Invention
The invention provides an activated carbon fiber and a method for loading carbon nanotubes, aiming at the problems in the prior art.
The purpose of the invention can be realized by the following technical scheme:
an activated carbon fiber and a method for loading carbon nano tubes, the method comprises the following steps:
(1) and (3) activation: weighing 5mL of DMF solution, adding 0.75g of powdered potassium hydroxide and 0.25g of doping source, and dissolving in 50mL of deionized water to obtain a mixed solution; weighing 1g of fiber, immersing the fiber in the mixed solution, reacting for 2 hours in a water bath kettle with a constant temperature of 100 ℃, taking out the fiber, performing irradiation treatment by using 60 Co-gamma rays with the irradiation dose of 1kGy, taking out the fiber, immersing for 24 hours, taking out the fiber, washing to be neutral, and drying;
(2) pre-oxidation: putting the sample dried in the step (1) into a microwave oven, and staying for 10 minutes at 150w power and 10 minutes at 300w power;
(3) carbonizing: putting the fibers subjected to preoxidation treatment into a TL1200 tubular furnace, reacting in a nitrogen environment, controlling the temperature rise rate to be 5 ℃/min, carbonizing at 650 ℃ for 70min, and keeping the air pressure between 0.01MPa and 0.02MPa in the process;
(4) modified carbon fiber loaded precursor: weighing 0.5g of ferric acetylacetonate, adding into 50mL of polyalcohol solvent, and mechanically stirring for 4 hours to obtain a uniformly dispersed solution; then adding the carbon fiber subjected to surface carbonization, and mechanically stirring for 1h to obtain uniform carbon fiber/ferric acetylacetonate/polyalcohol solution; in N2Heating under protection, reacting at 150 deg.C for 2h, removing heat source, and reacting under N2Naturally cooling to room temperature under protection, washing for 3 times by using absolute ethyl alcohol, and drying for 24 hours in a vacuum drying oven at 60 ℃ to obtain a precursor-loaded carbon fiber sample;
(5) carbon nanotube-activated carbon fiber: weighing a carbon fiber sample loaded with a precursor, placing the sample in a chemical vapor deposition furnace, and performing chemical vapor deposition on the sample in N2And H2Heating to 450 ℃ at a heating rate of 5 ℃/min, and reducing for 40min at the temperature; in N2And H2Heating to 800 ℃ at a heating rate of 5 ℃/min, namely the growth temperature of the carbon nano tube, and simultaneously introducing C2H2Gas, growing carbon nano-tube for 2H, and stopping introducing H2And C2H2Gas in N2At a rate of 1.0cm3/cm3Cooling to room temperature under min conditions.
The technical scheme of the invention is as follows: the doping source in the step (1) is MSO or melamine.
The technical scheme of the invention is as follows: in the step (2), the polyalcohol solvent is pentaerythritol or glycerol.
The invention has the beneficial effects that:
the invention adopts a novel physical and chemical activation method (irradiation-chemical method) to prepare the activated carbon fiber. The method adopts a 60 Co-gamma ray irradiation method for activation, and simultaneously combines a conventional chemical method to prepare an activated carbon fiber product, thereby realizing the purpose of surface modification of the activated carbon fiber, and loading carbon nanotubes on the surface of the activated carbon fiber while surface modification of the activated carbon fiber is carried out, thereby further optimizing the structure and performance of the activated carbon fiber.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention:
example 1
(1) And (3) activation: weighing 5mL of DMF solution, adding 0.75g of potassium hydroxide ground into powder and a certain amount of doping source 0.25g (DMSO), and dissolving in 50mL of deionized water; weighing 1g of fiber, reacting for 2h in a constant temperature water bath kettle at 100 ℃, taking out, performing irradiation treatment by using 60 Co-gamma rays with the irradiation dose of 1kGy, and taking out and dipping for 24 h. Taking out, washing to be neutral, and drying.
(2) Pre-oxidation: the impregnated sample was weighed and placed in a microwave oven at 150w power for 10 minutes and 300w power for 10 minutes.
(3) Carbonizing: putting the fiber subjected to preoxidation treatment into a TL1200 tubular furnace, reacting in a nitrogen environment, controlling the temperature rise rate to be 5 ℃/min, carbonizing at 650 ℃ for 70min, and keeping the air pressure between 0.01MPa and 0.02MPa in the process.
(4) Modified carbon fiber loaded precursor: 0.5g of iron acetylacetonate (Fe (acac)3) Added to 50mL of a polyol solvent (pentaerythritol) and mechanically stirred for 4 hours to obtain a uniformly dispersed solution. Then adding the carbon fiber subjected to surface carbonization, and mechanically stirring for 1h to obtain uniform carbon fiber/ferric acetylacetonate/polyalcohol solution. In N2Heating under protection, reacting at 150 deg.C for 2h, removing heat source, and reacting under N2And naturally cooling to room temperature under protection, washing for 3 times by using absolute ethyl alcohol, and drying for 24 hours in a vacuum drying oven at 60 ℃ to obtain the precursor-loaded carbon fiber sample.
(5) Carbon nanotube-activated carbon fiber: weighing a carbon fiber sample loaded with a precursor, placing the sample in a chemical vapor deposition furnace, and performing chemical vapor deposition on the sample in N2And H2Is heated to the temperature of 450 ℃ at the heating rate of 5 ℃/min and is reduced for 40min at the temperature. In N2And H2Heating to 800 ℃ at a heating rate of 5 ℃/min, namely the growth temperature of the carbon nano tube, and simultaneously introducing C2H2Gas, growing carbon nano-tube for 2H, and stopping introducing H2And C2H2Gas in N2At a rate of 1.0cm3/cm3Cooling to room temperature under min conditions.
And (3) performance detection:
the fiber is irradiated and activated by 60 Co-gamma rays, when the irradiation dose is 1.2kGy, the prepared activated carbon fiber has excellent structural performance, and meanwhile, the surface of the activated carbon fiber is loaded with the carbon nano tube. The prepared activated carbon fiber-carbon nano tube product has larger specific surface area, stronger adsorption capacity, better chemical stability and environmental friendliness, and has huge application prospect in the fields of air purification, water treatment and the like.
Claims (3)
1. An activated carbon fiber and a method for loading carbon nano tubes are characterized in that: the method comprises the following steps:
(1) and (3) activation: weighing 5mL of DMF solution, adding 0.75g of powdered potassium hydroxide and 0.25g of doping source, and dissolving in 50mL of deionized water to obtain a mixed solution; weighing 1g of fiber, immersing the fiber in the mixed solution, reacting for 2 hours in a water bath kettle with a constant temperature of 100 ℃, taking out the fiber, performing irradiation treatment by using 60 Co-gamma rays with the irradiation dose of 1kGy, taking out the fiber, immersing for 24 hours, taking out the fiber, washing to be neutral, and drying;
(2) pre-oxidation: putting the sample dried in the step (1) into a microwave oven, and staying for 10 minutes at 150w power and 10 minutes at 300w power;
(3) carbonizing: putting the fibers subjected to preoxidation treatment into a TL1200 tubular furnace, reacting in a nitrogen environment, controlling the temperature rise rate to be 5 ℃/min, carbonizing at 650 ℃ for 70min, and keeping the air pressure between 0.01MPa and 0.02MPa in the process;
(4) modified carbon fiber loaded precursor: weighing 0.5g of ferric acetylacetonate, adding into 50mL of polyalcohol solvent, and mechanically stirring for 4 hours to obtain a uniformly dispersed solution; then adding the carbon fiber subjected to surface carbonization, and mechanically stirring for 1h to obtain uniform carbon fiber/ferric acetylacetonate/polyalcohol solution; in N2Heating under protection, reacting at 150 deg.C for 2h, and movingRemoving heat source at N2Naturally cooling to room temperature under protection, washing for 3 times by using absolute ethyl alcohol, and drying for 24 hours in a vacuum drying oven at 60 ℃ to obtain a precursor-loaded carbon fiber sample;
(5) carbon nanotube-activated carbon fiber: weighing a carbon fiber sample loaded with a precursor, placing the sample in a chemical vapor deposition furnace, and performing chemical vapor deposition on the sample in N2And H2Heating to 450 ℃ at a heating rate of 5 ℃/min, and reducing for 40min at the temperature; in N2And H2Heating to 800 ℃ at a heating rate of 5 ℃/min, namely the growth temperature of the carbon nano tube, and simultaneously introducing C2H2Gas, growing carbon nano-tube for 2H, and stopping introducing H2And C2H2Gas in N2At a rate of 1.0cm3/cm3Cooling to room temperature under min conditions.
2. The activated carbon fiber and the method for loading carbon nanotubes according to claim 1, wherein: the doping source in the step (1) is MSO or melamine.
3. The activated carbon fiber and the method for loading carbon nanotubes according to claim 1, wherein: in the step (2), the polyalcohol solvent is pentaerythritol or glycerol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011165492.1A CN114481365A (en) | 2020-10-27 | 2020-10-27 | Activated carbon fiber and method for loading carbon nano tube |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011165492.1A CN114481365A (en) | 2020-10-27 | 2020-10-27 | Activated carbon fiber and method for loading carbon nano tube |
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| Publication Number | Publication Date |
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| CN114481365A true CN114481365A (en) | 2022-05-13 |
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| CN202011165492.1A Pending CN114481365A (en) | 2020-10-27 | 2020-10-27 | Activated carbon fiber and method for loading carbon nano tube |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115672271A (en) * | 2022-10-25 | 2023-02-03 | 山东格瑞德环保科技有限公司 | Modified activated carbon for oil gas recovery and preparation method thereof |
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2020
- 2020-10-27 CN CN202011165492.1A patent/CN114481365A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115672271A (en) * | 2022-10-25 | 2023-02-03 | 山东格瑞德环保科技有限公司 | Modified activated carbon for oil gas recovery and preparation method thereof |
| CN115672271B (en) * | 2022-10-25 | 2023-12-15 | 山东格瑞德环保科技有限公司 | Modified activated carbon for oil gas recovery and preparation method thereof |
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Application publication date: 20220513 |