CN115594162A - Porous carbon wave-absorbing material and preparation method and application thereof - Google Patents
Porous carbon wave-absorbing material and preparation method and application thereof Download PDFInfo
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- CN115594162A CN115594162A CN202211090860.XA CN202211090860A CN115594162A CN 115594162 A CN115594162 A CN 115594162A CN 202211090860 A CN202211090860 A CN 202211090860A CN 115594162 A CN115594162 A CN 115594162A
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Abstract
The invention discloses a porous carbon wave-absorbing material and a preparation method and application thereof, belonging to the field of electromagnetic wave-absorbing materials. A method for producing a porous carbon material, comprising the steps of: under the protection of inert gas, coal tar pitch is dissolved in a carbon tetrachloride crosslinking agent, and then AlCl is added 3 Carrying out Friedel-Crafts reaction by using a catalyst to obtain a precipitate; and washing, extracting and drying the precipitate, and heating the obtained product under the protection of inert gas to obtain the porous carbon wave-absorbing material. Compared with the prior art, the invention utilizes coal pitch as a carbon source, prepares the hypercrosslinked microporous polymer material with high specific surface area by weaving aromatic compounds in the pitch through mild one-step Friedel-Crafts reaction, controls pyrolysis parameters to carry out high-temperature carbonization on the hypercrosslinked microporous polymer material, prepares the coal pitch-based derivative porous carbon wave-absorbing material, realizes a green, simple and economic porous carbon material preparation technology, and provides a new idea for preparing the wave-absorbing material at low cost.
Description
Technical Field
The invention relates to the field of electromagnetic wave absorbing materials, in particular to a porous carbon wave absorbing material and a preparation method and application thereof.
Background
The electromagnetic wave absorbing material can effectively absorb and protect electromagnetic waves, so that the electromagnetic wave absorbing material is widely used in practical application. In recent years, a porous carbon material is taken as one of carbon-based wave-absorbing materials, and is considered as an ideal material for preparing a high-performance electromagnetic wave-absorbing material due to the characteristics of ultralow density, rich pore structure, large specific surface area, excellent dielectric loss capacity and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a porous carbon wave-absorbing material and a preparation method and application thereof.
The purpose of the invention can be realized by the following technical scheme:
a method for producing a porous carbon material, comprising the steps of:
under the protection of inert gas, coal tar pitch is dissolved in a carbon tetrachloride cross-linking agent, and then an AlCl3 catalyst is added to carry out Friedel-Crafts reaction to obtain a precipitate;
and washing, extracting and drying the precipitate, and heating the obtained product under the protection of inert gas to obtain the porous carbon wave-absorbing material.
Optionally, the heating conditions are as follows: the resulting product was heated to 700 ℃ at a 5 ℃/minute ramp rate.
Optionally, the detergent used in the washing process comprises ethanol.
Optionally, the extraction step is: the mixture was extracted with ethanol and dichloromethane, respectively, in a soxhlet extractor.
Optionally, the inert gas is argon.
The invention has the beneficial effects that:
the preparation method provided by the invention has the advantages that coal pitch is used as a carbon source, the aromatic compounds in the pitch are woven through a mild one-step Friedel-Crafts reaction to prepare the super-crosslinked microporous polymer material with a high specific surface area, pyrolysis parameters are controlled to carry out high-temperature carbonization on the super-crosslinked microporous polymer material, the coal pitch-based derived porous carbon wave-absorbing material is prepared, a green, simple and economic porous carbon material preparation technology is realized, and a new thought is provided for preparing the wave-absorbing material at low cost.
Drawings
The invention will be further described with reference to the accompanying drawings.
Fig. 1 shows the electromagnetic wave reflection loss of the porous carbon wave-absorbing material prepared in the embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The coal tar pitch is a complex mixture composed of polycyclic aromatic hydrocarbons, can be regarded as a basic structural unit of a graphite carbon material on the molecular layer surface, and contains a large amount of polycyclic aromatic hydrocarbons and heterocyclic compounds of elements such as O, N, S and the like, wherein part of the aromatic hydrocarbons can be easily subjected to thermal polycondensation at high temperature to form aromatic hydrocarbon planar molecules, and the macromolecules are stacked into a liquid-state-to-solid-state transition laminated body through intermolecular force to form the porous carbon microspheres under the action of surface energy. Meanwhile, the obtained porous carbon material has high conductivity due to rich polycyclic aromatic hydrocarbons in the coal pitch, and more importantly, the coal pitch has the characteristics of low molecular weight, high carbon content, high aromaticity and polymerization degree, relatively low content of heteroatoms and metals and the like, so that high yield and low cost can be realized. By Friedel-Crafts reaction to weave the low functionality rigid aromatic compound in the asphalt, the microporous polymer network with high specific surface area is synthesized efficiently in one step.
Specifically, coal tar pitch is first dissolved in carbon tetrachloride crosslinking agent in argon atmosphere and certain amount of AlCl is then added 3 Allowing the catalyst to react at 58 ℃ for 24h, washing the obtained precipitate with ethanol three times, and then respectivelyThe extract was extracted with ethanol and dichloromethane for 12 hours in a soxhlet extractor and finally the resulting powder was dried at 80 ℃ under reduced pressure for 24h. And placing the obtained powder in a tube furnace, and keeping the temperature of the tube furnace at 700 ℃ for 4 hours at the heating rate of 5 ℃/min in the argon atmosphere to obtain the coal tar pitch derived porous carbon material.
Because the aromatic compound content in the coal pitch is high, the porous carbon material can be prepared with high yield and low cost through Friedel-Crafts reaction; meanwhile, the inherent heteroatoms such as S, N and the like and the primary defects in the coal pitch can be reserved after carbonization and combined with the porous carbon framework, and rich interface polarization and dipole polarization sites can be provided, so that the electromagnetic wave absorption performance is improved. The prepared hypercrosslinked polymer has considerable micropore network structure and specific surface area up to 588m 2 (iv) g; after high-temperature carbonization, the prepared porous carbon material has rich porous structure and reasonable pore size distribution, can endow the material with good impedance matching and prolong the transmission path of electromagnetic waves, is favorable for multiple reflection and scattering of the electromagnetic waves in the material, increases the attenuation of the electromagnetic waves, has the lowest reflection coefficient of about-54.9 dB and the effective wave absorption range of 5.1GHz (as shown in figure 1), and can realize the effective absorption of the electromagnetic waves.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (7)
1. A method for producing a porous carbon material, characterized by comprising the steps of:
under the protection of inert gas, coal tar pitch is dissolved in a carbon tetrachloride crosslinking agent, and then AlCl is added 3 Carrying out Friedel-Crafts reaction by using a catalyst to obtain a precipitate;
and washing, extracting and drying the precipitate, and heating the obtained product under the protection of inert gas to obtain the porous carbon wave-absorbing material.
2. The method for producing a porous carbon material according to claim 1, wherein the heating conditions are: the resulting product was heated to 700 ℃ at a 5 ℃/minute ramp rate.
3. The method according to claim 1, wherein the washing agent used in the washing step comprises ethanol.
4. The method for producing a porous carbon material according to claim 1, wherein the extraction step comprises: the extract was extracted with ethanol and dichloromethane, respectively, in a soxhlet extractor.
5. The method for producing a porous carbon material according to claim 1, wherein the inert gas is argon gas.
6. A porous carbon material obtained by the production method according to any one of claims 1 to 5.
7. Use of the porous carbon material of claim 6 in a wave absorbing device or coating.
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| CN202211090860.XA CN115594162A (en) | 2022-09-07 | 2022-09-07 | Porous carbon wave-absorbing material and preparation method and application thereof |
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| CN202211090860.XA CN115594162A (en) | 2022-09-07 | 2022-09-07 | Porous carbon wave-absorbing material and preparation method and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE771973A (en) * | 1970-09-08 | 1971-12-31 | Coal Industry Patents Ltd | PROCESS FOR THE MANUFACTURING OF CARBON FIBERS, FILAMENTS AND FILMS |
| CN104300150A (en) * | 2014-05-07 | 2015-01-21 | 河南中联高科新能源有限公司 | Asphalt-based nanoporous carbon material, negative material thereof, and lithium ion battery |
| CN106206066A (en) * | 2016-07-13 | 2016-12-07 | 洛阳力容新能源科技有限公司 | Epoxy resin-matrix porous carbon materials, absorbent charcoal composite material, preparation method and application |
| CN111232973A (en) * | 2020-03-06 | 2020-06-05 | 安徽马钢化工能源科技有限公司 | Method for preparing coal tar pitch-based activated porous carbon through chloride mixture melting and alkali activation |
-
2022
- 2022-09-07 CN CN202211090860.XA patent/CN115594162A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE771973A (en) * | 1970-09-08 | 1971-12-31 | Coal Industry Patents Ltd | PROCESS FOR THE MANUFACTURING OF CARBON FIBERS, FILAMENTS AND FILMS |
| CN104300150A (en) * | 2014-05-07 | 2015-01-21 | 河南中联高科新能源有限公司 | Asphalt-based nanoporous carbon material, negative material thereof, and lithium ion battery |
| CN106206066A (en) * | 2016-07-13 | 2016-12-07 | 洛阳力容新能源科技有限公司 | Epoxy resin-matrix porous carbon materials, absorbent charcoal composite material, preparation method and application |
| CN111232973A (en) * | 2020-03-06 | 2020-06-05 | 安徽马钢化工能源科技有限公司 | Method for preparing coal tar pitch-based activated porous carbon through chloride mixture melting and alkali activation |
Non-Patent Citations (2)
| Title |
|---|
| 李思雨，邹冲等: "Friedel-Crafts交联沥青基纳米孔炭材料的制备及电化学性能", 中国化学会第14届反应性高分子学术讨论会, pages 35 - 36 * |
| 马豪等: "AlCl3催化中温煤沥青制备中间相炭微球的研究", 炭素技术, vol. 38, no. 4, pages 32 - 36 * |
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