CN115092927B - Carbon fiber composite resin-based activated carbon and preparation method thereof - Google Patents
Carbon fiber composite resin-based activated carbon and preparation method thereof Download PDFInfo
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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 resin-based activated carbon comprises the following steps: (1) resin depolymerization: depolymerizing the carbon fiber composite resin by adopting a nitric acid oxidation method to obtain a depolymerized product; (2) resin activation: and adding the depolymerized product into a phosphoric acid solution, stirring and soaking, drying, and activating under an inert atmosphere to obtain the carbon fiber composite 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 waste resin-based activated carbon, adopts a phosphoric acid activation method to prepare resin-based activated carbon, and has the characteristics of high specific surface area, high pore content and phosphorus element doping, thereby providing possibility for realizing high value of waste composite material resin.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to carbon fiber composite resin-based activated carbon and a preparation method thereof.
Background
The carbon fiber composite resin (carbon fiber composite for short) is widely applied to important fields such as aerospace, new energy automobiles, wind power, medical equipment and the like. In recent years, with the use of carbon fiber composites 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 on which the carbon fiber composite material depends for survival is seriously damaged. Therefore, how to treat the waste carbon fiber composite material becomes a current problem to be solved urgently. At present, researchers have developed many techniques for recycling waste carbon fiber composite materials, such as a solvent dissociation method, a pyrolysis method, a supercritical fluid, a fluidized bed method, and the like, but the current recycling techniques only can obtain reusable carbon fibers, and cannot realize the recycling and the utilization of resins.
The raw materials for preparing the active carbon are mainly biomass materials, such as coconut shells, straws, wood and the like. The active carbon material with high specific surface area and porosity is obtained by chemical reaction of the raw materials and the 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 are available. For example, yan et al prepared carbon nanoplatelets having a multi-stage pore size distribution of macropores, mesopores, and micropores, which have an ultra-high specific surface area, by one-step carbonization and activation using a mixture of a water-soluble phenolic resin and KOH. Zhang et al similarly used water-soluble phenolic resin as carbon precursor and Na 2 CO 3 As an activator, nitrogen was introduced to carry out carbonization. Finally, the three-dimensional porous structure active carbon with high purity, high carbon yield and excellent conductivity is obtained. Dong et al uses phenolic resin as a carbon source, ethanol as a solvent and hexamethylenetetramine as a curing agent, and uses potassium ferrite as an activating agent for carbonization to obtain the carbon material with a flexible porous structure with large specific surface area and high graphitization degree. However, the existing technology for recycling the carbon fiber composite material can pollute the environment through a landfill method and a thermal decomposition method, the landfill method can pollute the environment, the thermal decomposition method breaks down the resin, and the remaining carbon fiber can be reused but the resin is wasted) is used as a raw material, and the research on preparing the activated carbon through chemical activation is not reported yet.
Disclosure of Invention
The invention aims to provide carbon fiber composite resin-based activated carbon and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the above object, the present invention provides the following solutions:
one of the technical schemes of the invention is as follows: the preparation method of the carbon fiber composite resin-based activated carbon comprises the following steps:
(1) Resin depolymerization: depolymerizing the carbon fiber composite resin by adopting a nitric acid oxidation method to obtain a depolymerized product;
the carbon fiber composite resin is a waste carbon fiber composite.
The resin depolymerization can effectively separate the carbon fiber from the resin, the carbon fiber can be reused, and the separated resin can be carbonized to prepare the activated carbon.
(2) Resin activation: and adding the depolymerized product into a phosphoric acid solution, stirring and soaking, drying, and activating under an inert atmosphere to obtain the carbon fiber composite resin-based activated carbon.
The carbon material is due to the presence of SP 2 The hybridized carbon atoms show inertia, hydrophobicity and non-hydrophilicity, and the P element exists after phosphoric acid is used for activation, so that the specific surface area of the carbon material is increased, the pore structure is enriched, the active site is increased, and the activity of the carbon material is further improved.
Further, the resin depolymerization specifically includes: mixing the carbon fiber composite resin with a nitric acid aqueous solution, heating and refluxing for reaction, and distilling until no liquid residue exists, thereby obtaining the depolymerization product.
Further, the mass ratio of the carbon fiber composite resin to the nitric acid aqueous solution is 1:5 to 10; the concentration of the aqueous nitric acid solution is 50wt.%; the temperature of the heating reflux reaction is 100 ℃.
Further, the phosphoric acid solution has a concentration of 30 to 60wt.%.
Further, the mass/volume ratio of the depolymerization product and the phosphoric acid solution is 1g: 2-25 mL.
Further, the stirring and soaking 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 is activated, the method further comprises the steps of washing, drying and grinding the depolymerized product into powder, and specifically comprises the following steps: washing with water to pH 6-8, drying at 50-80 deg.c for 2-6 hr, and grinding into powder.
Further, the inert atmosphere is nitrogen or argon; the flow rate of the inert atmosphere is 2-5 m/s.
The second technical scheme of the invention is as follows: the carbon fiber composite resin-based activated carbon prepared by the preparation method.
The third technical scheme of the invention: an application of the carbon fiber composite resin-based activated carbon in the preparation of an adsorption material.
The invention discloses the following technical effects:
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 waste resin-based activated carbon, adopts a phosphoric acid activation method to prepare resin-based activated carbon, and has high specific surface area (640-990 m) 2 Per g) and a high pore content (total pore volume of 0.48 to 0.82 cm) 3 And/g) and phosphorus element doping (doping amount is 0.5-4.3%). 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 that are 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a transmission electron microscope image of activated carbon prepared in example 2 of the present invention;
FIG. 2 is a scanning electron microscope image of the activated carbon prepared in example 2 of the present invention;
FIG. 3 is a scanning electron microscope image of the activated carbon prepared in example 4 of the present invention;
FIG. 4 is a scanning electron microscope image of the activated carbon prepared in comparative example 1 of the present invention;
FIG. 5 is a graph showing the isothermal adsorption and desorption of nitrogen from the activated carbon prepared in examples 1 to 5 and comparative example 1 according to the present invention;
FIG. 6 shows the X-ray photoelectron spectra of the activated carbon prepared in examples 1 to 5 and comparative example 1 of the present invention.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions 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 this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 for the purpose of disclosing and describing the methods and materials associated with the documents. 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 invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
The carbon fiber composite resin adopted in the following examples of the present invention is a waste carbon fiber composite material, and the content of the resin in the material is 30 to 50wt.%.
Example 1
The preparation method of the carbon fiber composite 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 the three-neck flask to 100 ℃ by an oil bath for reflux reaction, cooling the carbon fiber composite material resin to room temperature after the carbon fiber composite material resin is completely dissolved, and distilling until no liquid remains to obtain a depolymerized product.
(2) Washing and drying of the resin: the depolymerized product was washed with deionized water to a ph=7 or so, then dried in an oven at 60 ℃ for 4 hours, and ground into powder with a mortar to obtain depolymerized product powder (particle size 5 μm or so) with a yield of about 30%, i.e., 1g of carbon fiber composite resin was depolymerized to obtain 0.3g of depolymerized product powder.
(3) Activation of the resin: uniformly mixing depolymerized product powder and phosphoric acid solution (the concentration is 50 wt.%) according to the mass/volume ratio of 1g to 10mL, stirring and soaking for 10h, and then drying in an oven at 110 ℃ for 24h until the water is evaporated to dryness to obtain a soaked sample; the impregnated sample was placed in a tube furnace, activated by heating to 400 c at a heating rate of 5 c/min under nitrogen atmosphere (flow rate of 3 m/s) for 1h, then washed with distilled water to remove impurities, and dried at 100 c to obtain carbon fiber composite resin-based activated carbon (AC-400) having a yield of 50%, i.e., 1g of depolymerized product powder can produce 0.5g of activated carbon.
Example 2
The difference with example 1 is that the activation temperature in step (3) is 500 ℃, and the carbon fiber composite resin-based activated carbon (AC-500) is obtained, the transmission electron microscope image is shown in FIG. 1, and the scanning electron microscope image 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 is 41%.
Example 3
The difference from example 1 is that the activation temperature in step (3) is 600℃to obtain carbon fiber composite resin-based activated carbon (AC-600).
The yield of the carbon fiber composite resin-based activated carbon is 36%.
Example 4
The difference from example 1 is that the activation temperature in step (3) is 700℃to obtain carbon fiber composite resin-based activated carbon (AC-700), and the scanning electron microscope image 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 is 33%.
Example 5
The difference from example 1 is that the activation temperature in the step (3) is 800℃to obtain carbon fiber composite resin-based activated carbon (AC-800).
The yield of the carbon fiber composite resin-based activated carbon is 31.3%.
Comparative example 1
The difference from example 1 is that step (3) specifically comprises: directly placing the resin powder into a tube furnace, heating to 800 ℃ at a heating rate of 5 ℃/min under nitrogen atmosphere (flow rate of 3 m/s) for activation, keeping for 1h, washing with distilled water to remove impurities, and drying at 100 ℃ to obtain carbon fiber composite resin-based active carbon (C-800), wherein a scanning electron microscope chart 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 is 30.7%.
Example 6
The preparation method of the carbon fiber composite 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 (concentration is 50 wt%) into a three-neck flask with a thermometer and a condensing reflux device according to a mass ratio of 1:5, heating 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 remains, thereby obtaining a depolymerized product.
(2) Washing and drying of the resin: the depolymerized product was washed with deionized water to ph=7 or so, then dried in an oven at 80 ℃ for 2 hours, and ground into powder with a mortar to obtain depolymerized product powder.
(3) Activation of the resin: uniformly mixing depolymerized product powder and phosphoric acid solution (the concentration is 30 wt.%) according to the mass/volume ratio of 1g to 25mL, stirring and soaking for 6h, and then drying for 24h in an oven at 110 ℃ until the water is evaporated to dryness to obtain a soaked sample; and (3) placing the immersed sample into a tube furnace, heating to 400 ℃ at a heating rate of 2 ℃/min under nitrogen atmosphere (the flow rate is 2 m/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 resin-based activated carbon.
The yield of the carbon fiber composite resin-based activated carbon is 48%.
Example 7
The preparation method of the carbon fiber composite 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 (concentration is 50 wt%) into a three-neck flask with a thermometer and a condensing reflux device according to a mass ratio of 1:10, heating 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 remains, thereby obtaining a depolymerized product.
(2) Washing and drying of the resin: the depolymerized product was washed with deionized water to ph=7 or so, then dried in an oven at 50 ℃ for 6 hours, and ground into powder with a mortar to obtain depolymerized product powder.
(3) Activation of the resin: uniformly mixing depolymerized product powder and phosphoric acid solution (with concentration of 60 wt.%) in a mass/volume ratio of 1g to 5mL, stirring and soaking for 12h, and then drying in an oven at 110 ℃ for 24h until water is evaporated to dryness to obtain a soaked sample; and (3) placing the immersed sample into a tube furnace, heating to 400 ℃ at a heating rate of 5 ℃/min under nitrogen atmosphere (the flow rate is 5 m/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 resin-based activated carbon.
The yield of the carbon fiber composite resin-based activated carbon is 48.5%.
According to research, 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 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 pore Performance data
TABLE 2 elemental content
As can be seen from table 2, as the activation temperature increases, the doping amount of the phosphorus element tends to increase and decrease, because at the activation temperature of 400 ℃ (AC-400), the phosphorus element doping is less and 500 ℃ (AC-500) is the optimal activation temperature due to the intersection of the activation temperature, so that not only the phosphorus element doping is more, but also the specific surface area is larger, and the performance of the activated carbon prepared at this time is the best. And the activation temperature is continuously increased, and the phosphorus element is reduced along with the decomposition of the small molecules.
The nitrogen adsorption and desorption properties of the activated carbon prepared in examples 1 to 5 and comparative example 1 were 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 the X-ray photoelectron spectra of the activated carbon prepared in examples 1 to 5 and comparative example 1.
As can be seen from fig. 6, the carbon content decreases, the nitrogen and oxygen content increases, the phosphorus content is highest at 500 c, and the phosphorus content decreases as the temperature continues to increase after phosphoric acid activation (as analyzed in connection with table 2).
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (6)
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 adopting a nitric acid oxidation method to obtain a depolymerized product;
(2) Resin activation: adding the depolymerized product into a phosphoric acid solution, stirring and soaking, drying, and activating under an inert atmosphere to obtain the carbon fiber composite resin-based activated carbon;
the concentration of the phosphoric acid solution is 30-60 wt.%;
the mass/volume ratio of the depolymerization product and the phosphoric acid solution is 1g: 2-25 mL;
the stirring and soaking time is 6-12 h;
the activation temperature is 400-800 ℃, the heating rate is 2-5 ℃/min, the time is 0.5-2 h, and the inert atmosphere is 2-5 m/s of nitrogen atmosphere.
2. The method for preparing carbon fiber composite resin-based activated carbon according to claim 1, wherein the resin depolymerization specifically comprises: mixing the carbon fiber composite resin with a nitric acid aqueous solution, heating and refluxing for reaction, and distilling until no liquid residue exists, thereby obtaining the depolymerization product.
3. The method for preparing the carbon fiber composite resin-based activated carbon according to claim 2, wherein the mass ratio of the carbon fiber composite resin to the nitric acid aqueous solution is 1:5 to 10; the concentration of the aqueous nitric acid solution is 50wt.%; the temperature of the heating reflux reaction is 100 ℃.
4. The method for preparing the carbon fiber composite resin-based activated carbon according to claim 1, further comprising the steps of washing, drying and grinding the depolymerized product into powder before the resin is activated, and specifically comprising the steps of: washing with water to pH 6-8, drying at 50-80 deg.c for 2-6 hr, and grinding into powder.
5. A carbon fiber composite resin-based activated carbon prepared by the preparation method of any one of claims 1 to 4.
6. Use of the carbon fiber composite resin-based activated carbon of claim 5 in the preparation of an adsorbent material.
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| 树脂基球形活性炭活化工艺研究及应用;李曰星;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;全文 * |
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