CN111017902A - Preparation method of three-dimensional continuous porous carbon material - Google Patents

Preparation method of three-dimensional continuous porous carbon material Download PDF

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CN111017902A
CN111017902A CN201911302577.7A CN201911302577A CN111017902A CN 111017902 A CN111017902 A CN 111017902A CN 201911302577 A CN201911302577 A CN 201911302577A CN 111017902 A CN111017902 A CN 111017902A
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sio
carbon material
porous carbon
continuous porous
dimensional continuous
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刘鹏
刘远
吴雯雯
储亚琪
宋月婵
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Shaanxi Normal University
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Shaanxi Normal University
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30

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Abstract

The invention discloses a preparation method of a three-dimensional continuous porous carbon material, which comprises the following steps of firstly, using SiO2Preparing SiO with a core-shell structure by using powder as a template and resorcinol and formaldehyde as precursors2The preparation method comprises the following steps of @ phenolic resin powder, hot pressing the obtained powder into a block, calcining under the protection of inert atmosphere, and finally corroding SiO by hydrofluoric acid2And obtaining the three-dimensional continuous porous carbon material. The raw materials adopted by the invention are simple and easy to obtain, the operation is simple and controllable, and the prepared three-dimensional continuous porous carbon material has regular appearance, uniform size and excellent microwave absorption performance.

Description

Preparation method of three-dimensional continuous porous carbon material
Technical Field
The invention belongs to the technical field of preparation of microwave absorbing materials, and particularly relates to a preparation method of a three-dimensional continuous porous carbon material.
Background
With the explosive development of electronic devices and microwave communication, electromagnetic noise reduction and stealth technologies are receiving wide attention. Microwave absorbing materials are a class of materials that substantially attenuate electromagnetic waves by absorbing them and converting them into heat or other forms of energy. The traditional wave-absorbing material mainly comprises magnetic metal materials such as Fe, Co, Ni and the like, Fe3O4、MnFe2O4、CoFe2O4、BaFe12O19And ferrite materials and carbonyl iron wave-absorbing materials. Due to the synergistic effect of the electric loss and the magnetic loss, the wave-absorbing material has better impedance matching, thereby having excellent microwave absorption performance and being practically applied in the military and civil fields. However, the large loading ratio, the poor chemical stability and the high density limit the applications to some extent. In comparison, the carbon-based wave-absorbing material has great potential in the aspect of preparing the strong absorption broadband wave-absorbing material due to the advantages of light weight, stable physicochemical property and adjustable dielectric loss. Numerous studies have shown that carbon materials with hierarchical porous structures exhibit greater effective absorption bandwidths. At present, the hierarchical porous structure carbon material capable of effectively absorbing microwaves is mainly derived from carbonization (J.xi, et al (2017) carbon.124,492-498; Z.Wu, et al (2018) ACS Appl MaterInterfaces.10,11108-11115; patent CN106744791A) of biological materials, but the artificially synthesized carbon material with the size-adjustable micro-nano hierarchical structure is rarely reported. And it has been reported that the pore diameter and pore wall thickness of porous carbon prepared in (j.wang, et al (2019) Chemical engineering journal.357,376-383 and g.zhang, et al (2019) Advanced Functional materials.29,1806722) are difficult to regulate, and if used as a wave absorbing agent, it is difficult to further regulate electromagnetic parameters to obtain the optimum microwave absorption performance.
Disclosure of Invention
The invention aims to provide a preparation method of a three-dimensional continuous porous carbon material which is cellular, regular in shape, uniform and adjustable in pore size and good in microwave absorption performance.
The preparation method of the three-dimensional continuous porous carbon material comprises the following steps:
1. mixing SiO2Adding the powder into a mixed solution with the volume ratio of organic solvent to water being more than 1:1, uniformly dispersing by ultrasonic, and then dropwise adding an alkaline solution to adjust the pH value to 7-14 or heating the solution to 25-100 ℃; then adding resorcinol and formaldehyde respectively, stirring for 10 min-36 h, and adding the mixture into SiO2Polymerizing phenolic resin on the surface in situ to form SiO with a core-shell structure2@ phenolic resin powder; wherein the organic solvent is any one of ethanol, acetone, glycol and glycol ether.
2. Adopting a hot pressing mode to carry out hot pressing on the SiO with the core-shell structure obtained in the step 12The @ phenolic resin powder is pressed into a block body, the pressure is controlled to be 100-500 MPa, the pressurizing temperature is controlled to be 120-400 ℃, the hot pressing time is controlled to be 10 min-2 h, and the three-dimensional SiO is obtained2@ C block.
3. Subjecting the three-dimensional SiO obtained in the step 22Calcining the @ C block at 500-1200 ℃ for 30 min-4 h in inert atmosphere, and then pickling with hydrofluoric acid to remove SiO2And obtaining the three-dimensional continuous porous carbon material.
In the step 1, SiO is preferably used2Adding the powder into a mixed solution of an organic solvent and water in a volume ratio of 2-10: 1, uniformly dispersing by ultrasonic, and then dropwise adding an alkaline solution to adjust the pH to 8-10; then adding resorcinol and formaldehyde respectively, stirring for 12-24 h, and adding the mixture into SiO2Polymerizing phenolic resin on the surface in situ to form SiO with a core-shell structure2@ phenolic resin powder. Wherein, the organic solvent is preferably ethanol.
In the above step 1, the SiO2The powder is spherical SiO with the particle size of 10-2000 nm2The alkaline solution is ammonia water, sodium hydroxide aqueous solution or potassium hydroxide aqueous solution.
In the step 1, the resorcinol, formaldehyde and SiO2The mass ratio of the powder is 1: (0.1-1.1): (0.6-30), preferably resorcinol, formaldehyde and SiO2The mass ratio of the powder is 1: (0.3-0.8) and (2-15).
In the step 2, the pressure of hot pressing is preferably 200-400 MPa, the temperature is 180-250 ℃, and the hot pressing time is 30 min-1 h.
In the step 3, the three-dimensional SiO obtained in the step 2 is preferably used2Calcining the @ C block body for 1-2 h at 600-1000 ℃ in an inert atmosphere.
The invention has the following beneficial effects:
the invention adopts the existing mature process, the process is simple and convenient, the operation is easy, the used raw materials are rich, the cost is low, the prepared honeycomb three-dimensional continuous porous carbon material has continuous pore distribution, the pore diameter and the pore wall size are uniform and adjustable, and the microwave absorbing material prepared by the material has larger effective absorption bandwidth, smaller wave absorber load ratio and higher reflection loss. Besides being used as microwave absorbing materials, the material also has important application prospect and economic value in the fields of lithium ion batteries, catalysis, drug delivery, gas sensors, supercapacitors and the like.
Drawings
FIG. 1 is SiO in example 12Powder (a) and SiO2@ phenolic resin powder (b), three-dimensional SiO2And section (C) of the @ C block and section (d) of the three-dimensional continuous porous carbon material.
Fig. 2 is a TEM image of the three-dimensional continuous porous carbon material prepared in example 1.
Fig. 3 is an XRD pattern of the three-dimensional continuous porous carbon material prepared in example 1.
Fig. 4 is a two-dimensional contour diagram (load ratio 8%) of the microwave absorbing performance of the three-dimensional continuous porous carbon material prepared in example 1.
Fig. 5 is an SEM image of a cross-section of the three-dimensional continuous porous carbon material prepared in example 2.
FIG. 6 is an SEM image of a cross-section of the three-dimensional continuous porous carbon material prepared in example 3.
Fig. 7 is an SEM image of a cross section of the three-dimensional continuous porous carbon material prepared in example 4.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
1. 3g of SiO with a particle size of about 600nm2Adding the powder into a mixed solvent of 400mL of ethanol and 100mL of water, ultrasonically dispersing for 1h, then dropwise adding ammonia water to adjust the pH value to 8, then adding 0.4g of resorcinol and 0.56g of formaldehyde aqueous solution with the mass concentration of 38%, magnetically stirring for 24h, centrifugally washing and drying to obtain SiO2@ phenolic resin powder.
2. 0.4g of SiO are weighed2@ phenolic resin powder, 0.1mL deionized water is added,grinding for 2min, pressing into sheet by hot pressing at 300MPa and 200 deg.C for 1h to obtain three-dimensional SiO2@ C block.
3. Mixing three-dimensional SiO2Heating the @ C block to 700 ℃ at a speed of 2 ℃/min under the atmosphere of high-purity argon, calcining the temperature at a constant temperature for 2h, and then pickling the temperature by adopting hydrofluoric acid with the mass concentration of 45 percent to remove SiO2And obtaining the three-dimensional continuous porous carbon material.
Respectively aligning the SiO with a scanning electron microscope2Powder, SiO2@ phenolic resin powder and three-dimensional SiO2The @ C block and the three-dimensional continuous porous carbon material are characterized, the result is shown in figure 1, the morphology of the prepared three-dimensional continuous porous carbon material is observed by adopting a field emission transmission electron microscope, and the result is shown in figure 2. As can be seen from FIGS. 1 and 2, the prepared carbon material has uniform and continuous pores, regular morphology and pore size of about 610 nm. FIG. 3 shows the results of X-ray diffraction measurements on the carbon material obtained in example 1, which shows its amorphous nature and low degree of graphitization; in order to illustrate the excellent properties of the prepared three-dimensional porous carbon material, the three-dimensional porous carbon material and paraffin are mixed according to the mass ratio of 8% to prepare a composite wave-absorbing sample, a vector network analyzer is adopted to test the electromagnetic parameters and the wave-absorbing performance of the composite wave-absorbing sample, and the result is shown in figure 4, so that the wave-absorbing material has good microwave absorption performance and has an effective absorption bandwidth (RL) of 8.2GHz when the coating is about 3.5mm<-10dB), the application potential is great.
Example 2
In step 1 of this example, SiO was used2The particle size of the powder was about 190nm, and the other steps were the same as in example 1, to obtain a three-dimensional continuous porous carbon material (see fig. 5).
Example 3
In step 1 of this example, SiO was used2The particle size of the powder was about 360nm, and the other steps were the same as in example 1, to obtain a three-dimensional continuous porous carbon material (see fig. 6).
Example 4
In step 1 of this example, SiO was used2The particle size of the powder was about 570nm, and the other steps were the same as in example 1And obtaining the three-dimensional continuous porous carbon material (see figure 7).
Example 5
In step 1 of this example, 3g of SiO with a particle size of about 600nm were added2Adding the powder into a mixed solvent of 400mL of ethanol and 100mL of water, ultrasonically dispersing for 1h, then dropwise adding ammonia water to adjust the pH value to 8, then adding 0.8g of resorcinol and 1.12g of formaldehyde aqueous solution with the mass concentration of 38%, magnetically stirring for 24h, centrifugally washing and drying to obtain SiO2@ phenolic resin powder. The other steps are the same as the example 1, and the three-dimensional continuous porous carbon material is obtained.
Example 6
In step 2 of this example, the pressing temperature was controlled at 240 ℃, and the three-dimensional continuous porous carbon material was obtained in the same manner as in example 1 except for the above steps.
Example 7
In step 2 of this example, the pressure was controlled at 400MPa, and the three-dimensional continuous porous carbon material was obtained in the same manner as in example 1 except for the steps.
Example 8
In step 2 of this example, the hot pressing time was controlled to 2h, and the other steps were the same as in example 1, to obtain a three-dimensional continuous porous carbon material.
Example 9
In the step 1 of the embodiment, ammonia water is not dripped to adjust the pH value, the reaction solution is heated to 60 ℃, the reaction is carried out for 6 hours by magnetic stirring, and other steps are the same as the step 1, so that the three-dimensional continuous porous carbon material is obtained.

Claims (9)

1. A preparation method of a three-dimensional continuous porous carbon material is characterized by comprising the following steps:
(1) mixing SiO2Adding the powder into a mixed solution with the volume ratio of organic solvent to water being more than 1:1, uniformly dispersing by ultrasonic, and then dropwise adding an alkaline solution to adjust the pH value to 7-14 or heating the solution to 25-100 ℃; then adding resorcinol and formaldehyde respectively, stirring for 10 min-36 h, and adding the mixture into SiO2Polymerizing phenolic resin on the surface in situ to form SiO with a core-shell structure2@ phenolic resin powder; wherein, the organic solventThe agent is any one of ethanol, acetone, glycol and ethylene glycol ethyl ether;
(2) adopting a hot pressing mode to carry out hot pressing on the SiO with the core-shell structure obtained in the step (1)2The @ phenolic resin powder is pressed into a block body, the pressure is controlled to be 100-500 MPa, the pressurizing temperature is controlled to be 120-400 ℃, the hot pressing time is controlled to be 10 min-2 h, and the three-dimensional SiO is obtained2@ C block;
(3) subjecting the three-dimensional SiO obtained in the step (2)2Calcining the @ C block at 500-1200 ℃ for 30 min-4 h in inert atmosphere, and then pickling with hydrofluoric acid to remove SiO2And obtaining the three-dimensional continuous porous carbon material.
2. The method for producing a three-dimensional continuous porous carbon material according to claim 1, characterized in that: in the step (1), SiO2Adding the powder into a mixed solution of an organic solvent and water in a volume ratio of 2-10: 1, uniformly dispersing by ultrasonic, and then dropwise adding an alkaline solution to adjust the pH to 8-10; then adding resorcinol and formaldehyde respectively, stirring for 12-24 h, and adding the mixture into SiO2Polymerizing phenolic resin on the surface in situ to form SiO with a core-shell structure2@ phenolic resin powder.
3. The method for producing a three-dimensional continuous porous carbon material according to claim 2, characterized in that: the organic solvent is ethanol.
4. The method for producing a three-dimensional continuous porous carbon material according to any one of claims 1 to 3, characterized in that: the SiO2The powder is spherical SiO with the particle size of 10-2000 nm2。
5. The method for producing a three-dimensional continuous porous carbon material according to any one of claims 1 to 3, characterized in that: the alkaline solution is ammonia water, sodium hydroxide aqueous solution or potassium hydroxide aqueous solution.
6. The method for producing a three-dimensional continuous porous carbon material according to any one of claims 1 to 3, characterized in thatIn the following steps: the resorcinol, formaldehyde and SiO2The mass ratio of the powder is 1: (0.1-1.1) and (0.6-30).
7. The method for producing a three-dimensional continuous porous carbon material according to claim 6, characterized in that: the resorcinol, formaldehyde and SiO2The mass ratio of the powder is 1: (0.3-0.8) and (2-15).
8. The method for preparing a three-dimensional continuous porous carbon material according to claim 1, characterized in that: in the step (2), the hot pressing pressure is 200-400 MPa, the temperature is 180-250 ℃, and the hot pressing time is 30 min-1 h.
9. The method for preparing a three-dimensional continuous porous carbon material according to claim 1, characterized in that: in the step (3), the three-dimensional SiO obtained in the step (2) is used2Calcining the @ C block body for 1-2 h at 600-1000 ℃ in an inert atmosphere.
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Cited By (2)

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CN115477548A (en) * 2022-09-01 2022-12-16 天津大学 Preparation method of self-supporting three-dimensional porous carbon foam
CN115548265A (en) * 2022-09-01 2022-12-30 天津大学 Preparation method of self-supporting three-dimensional porous carbon embedded nanocrystalline active material composite foam

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Publication number Priority date Publication date Assignee Title
CN115477548A (en) * 2022-09-01 2022-12-16 天津大学 Preparation method of self-supporting three-dimensional porous carbon foam
CN115548265A (en) * 2022-09-01 2022-12-30 天津大学 Preparation method of self-supporting three-dimensional porous carbon embedded nanocrystalline active material composite foam
CN115477548B (en) * 2022-09-01 2023-11-17 天津大学 Preparation method of self-supporting three-dimensional porous carbon foam

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