CN115092927A - Carbon fiber composite material resin-based activated carbon and preparation method thereof - Google Patents
Carbon fiber composite material resin-based activated carbon and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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Abstract
The invention discloses carbon fiber composite resin-based activated carbon and a preparation method thereof, and belongs to the technical field of waste resource utilization. The preparation method of the carbon fiber composite material resin-based activated carbon comprises the following steps: (1) resin depolymerization: depolymerizing the carbon fiber composite resin by a nitric acid oxidation method to obtain a depolymerized product; (2) resin activation: and adding the depolymerization product into a phosphoric acid solution, stirring and dipping, drying, and activating in an inert atmosphere to obtain the carbon fiber composite material resin-based activated carbon. The invention adopts a nitric acid oxidation method (chemical method) to effectively separate carbon fibers from resin in the carbon fiber composite material, provides possibility for preparing the waste resin-based activated carbon, adopts a phosphoric acid activation method to prepare the resin-based activated carbon, and the activated carbon has the characteristics of high specific surface area, high pore content and phosphorus element doping, thereby providing possibility for realizing high-valued waste composite material resin.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to carbon fiber composite material resin-based activated carbon and a preparation method thereof.
Background
The carbon fiber composite resin (short for carbon fiber composite) is widely applied to important fields of aerospace, new energy automobiles, wind power, medical equipment and the like. In recent years, with the use of carbon fiber composite materials in large quantities, waste materials are increasing. The carbon fiber composite material mainly comprises carbon fibers (reinforcement) and resin (reinforcement), and wastes of the carbon fiber composite material cannot be degraded under natural conditions, so that the natural ecological environment which we rely on for survival is seriously damaged. Therefore, how to treat the waste carbon fiber composite material becomes a difficult problem to be solved at present. At present, researchers have developed many techniques for recovering waste carbon fiber composite materials, such as a solvent dissociation method, a high-temperature pyrolysis method, a supercritical fluid method, a fluidized bed method, and the like, but the current recovery techniques can only obtain carbon fibers that can be reused, and cannot realize recovery and utilization of resins.
Currently, the raw materials for preparing the activated carbon are mainly biomass materials, such as coconut shells, straws, woods and the like. The activated carbon material with high specific surface area and porosity is obtained by the chemical reaction of raw materials and an activating agent at high temperature. Resin is a carbon-rich organic material, and reports on the preparation of activated carbon by using resin as a raw material have been provided. For example, Yan et al, using a mixture of water-soluble phenolic resin and KOH, through one-step carbonization and activation, prepare carbon nanosheets with a multi-level pore size distribution of macropores, mesopores and micropores, which have an ultra-high specific surface area. Zhang et al also use water-soluble phenolic resin as carbon precursor and Na 2 CO 3 As an activating agent, nitrogen gas was introduced for carbonization. Finally obtaining the three-dimensional porous structure activated carbon with high purity, high carbon yield and excellent conductivity. Dong et al uses phenolic resin asThe carbon material is a carbon source, ethanol is used as a solvent, hexamethylenetetramine is used as a curing agent, the mixture is cured, potassium ferrite is used as an activating agent, and carbonization is carried out to obtain the carbon material with a flexible porous structure with large specific surface area and high graphitization degree. However, studies on the preparation of activated carbon by chemical activation have not been reported, in which waste carbon fiber composites (carbon fiber composites mainly comprise carbon fibers as a reinforcement and resin as a matrix) are used as raw materials, and conventional techniques for recycling carbon fiber composites can be used by landfill or thermal decomposition, which causes environmental pollution, and the thermal decomposition decomposes the resin to leave carbon fibers which can be reused but wastes the resin).
Disclosure of Invention
The invention aims to provide a carbon fiber composite resin-based activated carbon and a preparation method thereof, aiming at solving the problems in the prior art.
In order to achieve the purpose, the invention provides the following scheme:
one of the technical schemes of the invention is as follows: the carbon fiber composite resin-based activated carbon and the preparation method thereof comprise the following steps:
(1) resin depolymerization: depolymerizing the carbon fiber composite resin by a nitric acid oxidation method to obtain a depolymerized product;
the carbon fiber composite resin is a waste carbon fiber composite material.
The carbon fiber and the resin can be effectively separated by the depolymerization of the resin, the carbon fiber can be recycled, and the separated resin can be carbonized to prepare the activated carbon.
(2) Resin activation: and adding the depolymerization product into a phosphoric acid solution, stirring and dipping, drying, and activating in an inert atmosphere to obtain the carbon fiber composite material resin-based activated carbon.
Carbon material due to the presence of SP 2 Hybridized carbon atom, exhibitThe carbon material is inert, hydrophobic and not hydrophilic, and P element exists after the carbon material is activated by phosphoric acid, so that the specific surface area of the carbon material is increased, the pore structure is enriched, the active sites are increased, and the activity of the carbon material is further improved.
Further, the resin depolymerization specifically includes: and mixing the carbon fiber composite resin with a nitric acid aqueous solution, heating for reflux reaction, and distilling until no liquid remains to obtain the depolymerized product.
Further, the mass ratio of the carbon fiber composite material resin to the nitric acid aqueous solution is 1: 5-10; the concentration of the aqueous nitric acid solution was 50 wt.%; the temperature of the heating reflux reaction was 100 ℃.
Further, the concentration of the phosphoric acid solution is 30-60 wt.%.
Further, the mass/volume ratio of the depolymerization product to the phosphoric acid solution is 1g: 2-25 mL.
Further, the stirring and dipping time is 6-12 h.
Further, the activation temperature is 400-800 ℃, the heating rate is 2-5 ℃/min, and the time is 0.5-2 h.
Further, before the resin activation, the steps of washing, drying and grinding the depolymerization product into powder are also included, and the method specifically comprises the following steps: washing with water until the pH value is 6-8, drying at 50-80 ℃ for 2-6 h, and grinding into powder.
Further, the inert atmosphere is nitrogen or argon; the flow velocity of the inert atmosphere is 2-5 m/s.
The second technical scheme of the invention is as follows: a carbon fiber composite material resin-based activated carbon prepared by the preparation method.
The third technical scheme of the invention is as follows: an application of the carbon fiber composite material resin-based activated carbon in the preparation of an adsorption material.
The invention discloses the following technical effects:
the invention adopts nitric acid oxidation method (chemical method) to effectively separate carbon fiber from resin in the carbon fiber composite material, provides possibility for preparing waste resin-based activated carbon, adopts phosphoric acid activation method to prepare resin-based activated carbon, and activated carbonHas a high specific surface area (640-990 m) 2 A/g) and a high pore content (total pore volume of 0.48 to 0.82 cm) 3 The doping amount is 0.5-4.3 percent. The method provides possibility for realizing high value of the waste composite resin.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a transmission electron micrograph of an activated carbon prepared according to example 2 of the present invention;
FIG. 2 is a scanning electron micrograph of an activated carbon prepared according to example 2 of the present invention;
FIG. 3 is a scanning electron micrograph of an activated carbon prepared according to example 4 of the present invention;
FIG. 4 is a scanning electron micrograph of an activated carbon prepared according to comparative example 1 of the present invention;
FIG. 5 is a nitrogen adsorption/desorption isotherm curve of the activated carbon prepared in examples 1 to 5 of the present invention and comparative example 1;
FIG. 6 shows X-ray photoelectron spectra of activated carbons prepared in examples 1 to 5 of the present invention and comparative example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in the present disclosure, it is understood that each intervening value, to the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and materials in connection with which they pertain. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The carbon fiber composite resin adopted in the following embodiment of the invention is a waste carbon fiber composite material, and the content of the resin in the material is 30-50 wt.%.
Example 1
The preparation method of the carbon fiber composite material resin-based activated carbon comprises the following steps:
(1) resin depolymerization: adding carbon fiber composite resin (waste carbon fiber composite material, the content of the resin is 40 wt.%) and nitric acid aqueous solution (the concentration is 50 wt.%) into a three-neck flask with a thermometer and a condensing reflux device according to the mass ratio of 1:10, heating in an oil bath to 100 ℃ for reflux reaction, cooling to room temperature after the carbon fiber composite resin is completely dissolved, and distilling until no liquid residue exists to obtain a depolymerized product.
(2) Washing and drying of the resin: the depolymerization product is washed with deionized water until the pH value is about 7, then the mixture is dried in an oven at 60 ℃ for 4h and ground into powder by a mortar, so that depolymerization product powder (about 5 mu m in particle size) is obtained with a yield of about 30%, i.e. about 0.3g of depolymerization product powder can be obtained by depolymerization of 1g of carbon fiber composite resin.
(3) Activation of the resin: uniformly mixing depolymerized product powder and a phosphoric acid solution (with the concentration of 50 wt.%) in a mass/volume ratio of 1g:10mL, stirring and soaking for 10 hours, and then placing in an oven for drying at 110 ℃ for 24 hours until the water is evaporated to dryness to obtain a soaked sample; and (3) putting the impregnated sample into a tube furnace, heating to 400 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere (the flow rate is 3m/s) for activation, keeping the temperature for 1h, washing with distilled water, removing impurities, and drying at 100 ℃ to obtain the carbon fiber composite material resin-based activated carbon (AC-400), wherein the yield of the carbon fiber composite material resin-based activated carbon is 50%, namely 1g of depolymerization product powder can produce 0.5g of activated carbon.
Example 2
The difference from example 1 is that the activation temperature in step (3) is 500 ℃ to obtain carbon fiber composite resin-based activated carbon (AC-500), and the transmission electron microscope is shown in FIG. 1, and the scanning electron microscope is shown in FIG. 2.
As can be seen from fig. 1 and 2, the activated carbon has a graphitized structure and a porous structure.
The yield of the carbon fiber composite resin-based activated carbon was 41%.
Example 3
The difference from example 1 is that the activation temperature in step (3) was 600 ℃ to obtain a carbon fiber composite resin-based activated carbon (AC-600).
The yield of the carbon fiber composite resin-based activated carbon was 36%.
Example 4
The difference from example 1 is that the activation temperature in step (3) was 700 ℃ to obtain carbon fiber composite resin-based activated carbon (AC-700), and the scanning electron micrograph is shown in FIG. 3.
As can be seen from fig. 3, the activated carbon has a porous structure.
The yield of the carbon fiber composite resin-based activated carbon was 33%.
Example 5
The difference from example 1 is that the activation temperature in step (3) was 800 ℃ to obtain a carbon fiber composite resin-based activated carbon (AC-800).
The yield of the carbon fiber composite resin-based activated carbon was 31.3%.
Comparative example 1
The difference from the example 1 is that the step (3) is specifically: and directly putting the resin powder into a tube furnace, heating to 800 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere (the flow rate is 3m/s) for activation, keeping the temperature for 1h, washing with distilled water to remove impurities, and drying at 100 ℃ to obtain the carbon fiber composite material resin-based activated carbon (C-800), wherein a scanning electron microscope picture is shown in figure 4.
As can be seen from fig. 4, the activated carbon has a porous structure and the pore size becomes large.
The yield of the carbon fiber composite resin-based activated carbon was 30.7%.
Example 6
The preparation method of the carbon fiber composite material resin-based activated carbon comprises the following steps:
(1) resin depolymerization: adding carbon fiber composite resin (waste carbon fiber composite material) and nitric acid aqueous solution (with the concentration of 50 wt.%) into a three-neck flask with a thermometer and a condensation reflux device according to the mass ratio of 1:5, heating in an oil bath to 100 ℃ for reflux reaction, cooling to room temperature after the carbon fiber composite resin is completely dissolved, and distilling until no liquid residue exists to obtain a depolymerized product.
(2) Washing and drying of the resin: the depolymerization product was washed with deionized water to a pH of about 7, then dried in an oven at 80 ℃ for 2 hours, and pulverized with a mortar to obtain a depolymerization product powder.
(3) Activation of the resin: uniformly mixing depolymerized product powder and a phosphoric acid solution (with the concentration of 30 wt.%) in a mass/volume ratio of 1g:25mL, stirring and soaking for 6 hours, and then placing in an oven to dry for 24 hours at 110 ℃ until the water is evaporated to dryness to obtain a soaked sample; and (3) putting the impregnated sample into a tube furnace, heating to 400 ℃ at a heating rate of 2 ℃/min under the nitrogen atmosphere (the flow rate is 2m/s) for activation, keeping the temperature for 2 hours, washing with distilled water to remove impurities, and drying at 100 ℃ to obtain the carbon fiber composite material resin-based activated carbon.
The yield of the carbon fiber composite resin-based activated carbon was 48%.
Example 7
The preparation method of the carbon fiber composite material resin-based activated carbon comprises the following steps:
(1) resin depolymerization: adding carbon fiber composite resin (waste carbon fiber composite material) and nitric acid aqueous solution (with the concentration of 50 wt.%) into a three-neck flask with a thermometer and a condensation reflux device according to the mass ratio of 1:10, heating in an oil bath to 100 ℃ for reflux reaction, cooling to room temperature after the carbon fiber composite resin is completely dissolved, and distilling until no liquid residue exists to obtain a depolymerized product.
(2) Washing and drying of the resin: the depolymerization product was washed with deionized water to a pH of about 7, then dried in an oven at 50 ℃ for 6 hours, and pulverized with a mortar to obtain a depolymerization product powder.
(3) Activation of the resin: uniformly mixing depolymerized product powder and a phosphoric acid solution (with the concentration of 60 wt.%) in a mass/volume ratio of 1g:5mL, stirring and soaking for 12h, and then placing in an oven for drying at 110 ℃ for 24h until the water is evaporated to dryness to obtain a soaked sample; and (3) putting the impregnated sample into a tube furnace, heating to 400 ℃ at the heating rate of 5 ℃/min under the nitrogen atmosphere (the flow rate is 5m/s) for activation, keeping the temperature for 0.5h, washing with distilled water to remove impurities, and drying at 100 ℃ to obtain the carbon fiber composite material resin-based activated carbon.
The yield of the carbon fiber composite resin-based activated carbon was 48.5%.
Researches show that the impregnation time of the depolymerized product powder in the phosphoric acid solution is less than 6 hours or more than 12 hours, and the performance of the prepared activated carbon is reduced compared with that of the activated carbon impregnated for 6-12 hours.
Effect example 1
The pore properties and the element contents of the activated carbons prepared in examples 1 to 5 and comparative example 1 were measured, and the results are shown in tables 1 and 2.
TABLE 1 well Performance data
TABLE 2 element content
As can be seen from Table 2, the doping amount of phosphorus element increases and then decreases with the increase of the activation temperature, because the activation temperature is 400 ℃ (AC-400), the doping amount of phosphorus element is less due to the low activation temperature, and 500 ℃ (AC-500) is the best activation temperature, so that the phosphorus element is more doped and the specific surface area is larger, and the performance of the prepared activated carbon is best. While continuing to increase the activation temperature, the phosphorus element decreases as the small molecules decompose.
The nitrogen adsorption/desorption performance of the activated carbon prepared in examples 1 to 5 and comparative example 1 was measured, and the results are shown in fig. 5.
As can be seen from fig. 5, AC-500 has the highest adsorption capacity and can be applied as a gas adsorbent, an electrode material, a dye adsorbent, etc.
FIG. 6 shows X-ray photoelectron spectra of activated carbons prepared in examples 1 to 5 and comparative example 1.
As can be seen from fig. 6, (analyzed in conjunction with table 2) the content of carbon element decreased, the content of nitrogen element and oxygen element increased, the content of phosphorus element was the highest at 500 ℃, and the content of phosphorus element decreased as the temperature continued to increase after phosphoric acid activation.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (10)
1. The preparation method of the carbon fiber composite resin-based activated carbon is characterized by comprising the following steps of:
(1) resin depolymerization: depolymerizing the carbon fiber composite resin by a nitric acid oxidation method to obtain a depolymerized product;
(2) resin activation: and adding the depolymerized product into a phosphoric acid solution, stirring, soaking, drying, and activating in an inert atmosphere to obtain the carbon fiber composite resin-based activated carbon.
2. The method for producing carbon fiber composite resin-based activated carbon as claimed in claim 1, wherein the depolymerization of the resin specifically comprises: and mixing the carbon fiber composite resin with a nitric acid aqueous solution, heating for reflux reaction, and distilling until no liquid remains to obtain the depolymerized product.
3. The method for producing a carbon fiber composite resin-based activated carbon as claimed in claim 2, wherein the mass ratio of the carbon fiber composite resin to the nitric acid aqueous solution is 1: 5-10; the concentration of the aqueous nitric acid solution is 50 wt.%; the temperature of the heating reflux reaction is 100 ℃.
4. The method for producing carbon fiber composite resin-based activated carbon as claimed in claim 1, wherein the concentration of the phosphoric acid solution is 30 to 60 wt.%.
5. The method for producing a carbon fiber composite resin-based activated carbon as claimed in claim 1, wherein the mass/volume ratio of the depolymerization product to the phosphoric acid solution is 1g: 2-25 mL.
6. The method for producing a carbon fiber composite resin-based activated carbon as claimed in claim 1, wherein the stirring and dipping time is 6 to 12 hours.
7. The method for producing a carbon fiber composite resin-based activated carbon as claimed in claim 1, wherein the activation temperature is 400 to 800 ℃, the temperature increase rate is 2 to 5 ℃/min, the time is 0.5 to 2 hours, and the inert atmosphere is a nitrogen atmosphere of 2 to 5 m/s.
8. The method of preparing carbon fiber composite resin-based activated carbon as claimed in claim 1, which further comprises the steps of washing, drying and pulverizing the depolymerization product before the resin activation, and specifically comprises: washing with water until the pH value is 6-8, drying at 50-80 ℃ for 2-6 h, and grinding into powder.
9. A carbon fiber composite resin-based activated carbon produced by the production method according to any one of claims 1 to 8.
10. Use of the carbon fiber composite resin-based activated carbon as claimed in claim 9 in the preparation of an adsorbent material.
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Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326897A (en) * | 2001-07-10 | 2001-12-19 | 中山大学 | Method for preparing porous carbon material with phenolic resin gel |
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| US20040097371A1 (en) * | 2002-11-19 | 2004-05-20 | Juzer Jangbarwala | Application of conductive adsorbents, activated carbon granules and carbon fibers as substrates in catalysis |
| JP2005294607A (en) * | 2004-04-01 | 2005-10-20 | Gun Ei Chem Ind Co Ltd | Electric double-layer capacitor using activated carbon fiber and its manufacturing method |
| JP2011074204A (en) * | 2009-09-30 | 2011-04-14 | Nippon Zeon Co Ltd | Method for recovering carbon fiber from carbon fiber-crosslinked resin composite material |
| CN103232615A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院山西煤炭化学研究所 | Method for degrading epoxy resin carbon fiber composite material |
| CN103451931A (en) * | 2012-06-04 | 2013-12-18 | 金发科技股份有限公司 | Carbon fiber surface modifier, modified carbon fiber, composite material, and preparation methods thereof |
| CN104030287A (en) * | 2014-07-09 | 2014-09-10 | 四川创越炭材料有限公司 | Spherical activated carbon and preparation method thereof |
| CN105384162A (en) * | 2015-12-04 | 2016-03-09 | 华南理工大学 | Corncob-based porous carbon material, and preparation method and application thereof |
| WO2017009662A1 (en) * | 2015-07-16 | 2017-01-19 | C-Tex Limited | Shaped nanoporous bodies |
| CN108440904A (en) * | 2018-02-07 | 2018-08-24 | 珠海诚然科技服务有限公司 | A kind of carbon fiber-reinforced resin dusty material |
| CN108640699A (en) * | 2018-04-28 | 2018-10-12 | 中国人民解放军国防科技大学 | Method for preparing carbon/carbon preformed body by recycling carbon fiber reinforced resin matrix composite material |
| JP2019064886A (en) * | 2017-10-04 | 2019-04-25 | 株式会社Kri | Method and system for recovering carbon-containing material |
| CN111185462A (en) * | 2020-01-16 | 2020-05-22 | 德州骏腾材料科技有限公司 | Recycling method of carbon fiber reinforced epoxy resin matrix composite material |
| CN113135567A (en) * | 2021-04-28 | 2021-07-20 | 安徽工程大学 | Preparation method of activated carbon and product thereof |
-
2022
- 2022-07-15 CN CN202210837469.5A patent/CN115092927B/en active Active
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326897A (en) * | 2001-07-10 | 2001-12-19 | 中山大学 | Method for preparing porous carbon material with phenolic resin gel |
| US20040097371A1 (en) * | 2002-11-19 | 2004-05-20 | Juzer Jangbarwala | Application of conductive adsorbents, activated carbon granules and carbon fibers as substrates in catalysis |
| CN1483754A (en) * | 2003-07-30 | 2004-03-24 | 哈尔滨工业大学 | Chenical recovery method for thermosetting epoxy compound material |
| JP2005294607A (en) * | 2004-04-01 | 2005-10-20 | Gun Ei Chem Ind Co Ltd | Electric double-layer capacitor using activated carbon fiber and its manufacturing method |
| JP2011074204A (en) * | 2009-09-30 | 2011-04-14 | Nippon Zeon Co Ltd | Method for recovering carbon fiber from carbon fiber-crosslinked resin composite material |
| CN103451931A (en) * | 2012-06-04 | 2013-12-18 | 金发科技股份有限公司 | Carbon fiber surface modifier, modified carbon fiber, composite material, and preparation methods thereof |
| CN103232615A (en) * | 2013-05-07 | 2013-08-07 | 中国科学院山西煤炭化学研究所 | Method for degrading epoxy resin carbon fiber composite material |
| CN104030287A (en) * | 2014-07-09 | 2014-09-10 | 四川创越炭材料有限公司 | Spherical activated carbon and preparation method thereof |
| WO2017009662A1 (en) * | 2015-07-16 | 2017-01-19 | C-Tex Limited | Shaped nanoporous bodies |
| CN105384162A (en) * | 2015-12-04 | 2016-03-09 | 华南理工大学 | Corncob-based porous carbon material, and preparation method and application thereof |
| JP2019064886A (en) * | 2017-10-04 | 2019-04-25 | 株式会社Kri | Method and system for recovering carbon-containing material |
| CN108440904A (en) * | 2018-02-07 | 2018-08-24 | 珠海诚然科技服务有限公司 | A kind of carbon fiber-reinforced resin dusty material |
| CN108640699A (en) * | 2018-04-28 | 2018-10-12 | 中国人民解放军国防科技大学 | Method for preparing carbon/carbon preformed body by recycling carbon fiber reinforced resin matrix composite material |
| CN111185462A (en) * | 2020-01-16 | 2020-05-22 | 德州骏腾材料科技有限公司 | Recycling method of carbon fiber reinforced epoxy resin matrix composite material |
| CN113135567A (en) * | 2021-04-28 | 2021-07-20 | 安徽工程大学 | Preparation method of activated carbon and product thereof |
Non-Patent Citations (8)
| Title |
|---|
| "石油化工科技期刊题录", no. 01 * |
| LEYVA-RAMOS, R ET AL.: "Adsorption of lead(II) from aqueous solution onto several types of activated carbon fibers" * |
| SHANG, TX ET AL.: "Oxygen- and nitrogen-co-doped activated carbon from waste particleboard for potential application in high-performance capacitance" * |
| 张敏敏: "酚醛树脂基活性炭材料的制备及其电化学性能" * |
| 张明;: "聚苯胺/酚醛树脂基活性炭复合材料的制备及表征", no. 02 * |
| 徐平来等: "碳纤维/环氧树脂复合材料低温化学法降解研究" * |
| 李曰星: "树脂基球形活性炭活化工艺研究及应用", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 李素敏: "结构—储能型碳纤维/环氧树脂基复合材料的制备及性能研究" * |
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