CN110482526B - Preparation method of biomass porous carbon electromagnetic wave-absorbing material with egg white as precursor - Google Patents

Preparation method of biomass porous carbon electromagnetic wave-absorbing material with egg white as precursor Download PDF

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CN110482526B
CN110482526B CN201910877416.4A CN201910877416A CN110482526B CN 110482526 B CN110482526 B CN 110482526B CN 201910877416 A CN201910877416 A CN 201910877416A CN 110482526 B CN110482526 B CN 110482526B
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porous carbon
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egg white
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CN110482526A (en
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刘宗林
彭庆宇
赫晓东
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Harbin Institute of Technology
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Abstract

A preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor belongs to the technical field of electromagnetic wave-absorbing material preparation. The method comprises the following steps: pretreating egg white to obtain a uniform protein solution; adding a potassium carbonate solution into the protein solution to form a uniform solution, titrating, and carrying out ultrasonic crushing to obtain a precursor solution; heating the precursor solution in water bath to obtain a porous carbon precursor; freezing with liquid nitrogen, and freeze-drying to obtain a dried porous carbon precursor; and heating and carbonizing the dried porous carbon precursor in an argon atmosphere. The invention widens the selection of carbon source materials of the porous carbon, and compared with other carbon source materials, the carbon source selected by the invention belongs to renewable biomass and has low cost. The porous carbon material has large specific surface area, and has a large number of active scattering sites due to the introduction of nitrogen elements, so that the porous carbon material has good electromagnetic wave absorbing performance.

Description

Preparation method of biomass porous carbon electromagnetic wave-absorbing material with egg white as precursor
Technical Field
The invention belongs to the technical field of electromagnetic wave-absorbing material preparation, and particularly relates to a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor.
Background
The electromagnetic wave absorbing material has become a hot point of research in the present following the continuous development of military (mainly applied to electromagnetic stealth of fighters, etc.) and civil (reducing the radiation of electromagnetic waves, etc. in consideration of human health) requirements.
The traditional electromagnetic wave-absorbing material is mainly ferromagnetic metal elements and oxides thereof, and although the wave-absorbing material has good absorption performance, the specific wave-absorbing capacity of the material is not very high due to the characteristic of high density of the metal elements. The novel electromagnetic wave-absorbing material represented by porous carbon solves the problems of poor mechanical flexibility, easy corrosion, complex processing and high cost of the metal element electromagnetic wave-absorbing material.
In recent years, the preparation technology of porous carbon tends to be perfect, and the application of the porous carbon in various fields also attracts the research interest of numerous scholars at home and abroad. The porous carbon material is a new research object in the field of electromagnetic wave absorption due to the advantages of light weight, porosity, high resistance consumption and the like.
Biomass is a carbon source material with rich content, and the doping of nitrogen element can be simply and efficiently solved through the carbonization of the biomass, so that the light, efficient and durable electromagnetic wave-absorbing material is obtained. However, the application of porous carbon in the field of electromagnetic wave absorption is still in the laboratory stage so far, and the application in large-scale engineering is not obtained, and in addition, the carbonization forming mechanism of the porous carbon material is still unknown. Although the wave absorbing capability of the porous carbon-based composite material is excellent, the contribution of the porous carbon matrix to electromagnetic wave absorption still has a space for improvement. The porous carbon material macroscopic body has the defects of poor microscopic pore structure design, incapability of batch production, poor structure designability and the like. Therefore, the structural design of the porous carbon material macroscopic body through different precursor selections, different preparation processes and the like has great research potential.
Disclosure of Invention
The invention aims to solve the problems of high density and low specific wave-absorbing strength of the existing electromagnetic wave-absorbing material, and provides a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor. Compared with other electromagnetic wave-absorbing materials, the biomass porous carbon material does not have subsequent doping of ferromagnetic metal elements in the preparation process, and the electromagnetic wave-absorbing material with low density and high wave-absorbing efficiency is prepared by using reproducible biomass egg white as a raw material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor comprises the following steps:
the method comprises the following steps: pretreatment of egg white: pretreating egg white by a physical dispersion mode to obtain a uniform protein solution;
step two: preparing a precursor solution: adding or not adding a potassium carbonate solution into the protein solution obtained in the step one to form a uniform solution, titrating with deionized water, and ultrasonically crushing the liquid by using an ultrasonic cell crusher to obtain a uniform precursor solution;
step three: preparation of the porous carbon precursor: heating the precursor solution obtained in the second step in a constant-temperature water bath to obtain a porous carbon precursor;
step four: drying the porous carbon precursor: freezing the porous carbon precursor obtained in the step three by using liquid nitrogen, and then carrying out freeze drying in a freeze dryer to obtain a dried porous carbon precursor;
step five, carbonization of the precursor: and heating and carbonizing the dried porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention widens the selection of carbon source materials of the porous carbon, and compared with other carbon source materials, the carbon source selected by the invention belongs to renewable biomass and has low cost. The porous carbon material has large specific surface area, and has a large number of active scattering sites due to the introduction of nitrogen elements, so that the porous carbon material has good electromagnetic wave absorbing performance.
2. The method has the advantages that the in-situ doping of nitrogen elements is realized by utilizing the protein, the cost is low, the steps are simple, a large amount of active scattering sites are generated inside the porous carbon material, and the electromagnetic wave absorption performance of the porous carbon is greatly improved.
3. The method realizes the nitrogen element doping of the porous carbon by adopting an in-situ doping mode, the electromagnetic wave absorption strength can reach more than 60dB when the thickness of the three-dimensional porous carbon material is less than 2mm, and the density is light and is 0.1-0.3 g/cm3
4. The biomass porous carbon material prepared by the invention has good electromagnetic wave-absorbing performance and lighter weight, and the electromagnetic wave-absorbing peak value reaches 60.67dB when the thickness of the porous carbon material is only 1.34mm, so that the biomass porous carbon material is an excellent electromagnetic wave-absorbing material.
Drawings
FIG. 1 is a graph showing the dielectric constant of biomass porous carbon obtained in example 2 as a function of frequency;
FIG. 2 is a graph showing the relationship between the magnetic permeability and the frequency of the biomass porous carbon obtained in example 2;
FIG. 3 is a schematic diagram of the dielectric loss tangent angle of the biomass porous carbon obtained in example 2;
FIG. 4 is a schematic diagram of magnetic loss tangent angle of biomass porous carbon obtained in example 2;
FIG. 5 is a 3D diagram showing the theoretical wave absorption value of the biomass porous carbon obtained in example 2;
FIG. 6 is a microstructure of fiber bundle-like structural features of the biomass porous carbon obtained in example 1;
FIG. 7 is a microscopic topography map of the multilevel porous structure-like features of the biomass porous carbon obtained in example 3;
FIG. 8 is a microscopic morphology of the biomass porous carbon obtained in example 1;
FIG. 9 is a microscopic morphology of the biomass porous carbon obtained in example 2;
fig. 10 is a microscopic morphology map of the biomass porous carbon obtained in example 3.
Detailed Description
The technical solutions of the present invention are further described below with reference to the drawings and the embodiments, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
The first embodiment is as follows: the embodiment describes a preparation method of a biomass porous carbon electromagnetic wave-absorbing material with egg white as a precursor, which comprises the steps of heating egg white and potassium carbonate as raw materials according to the thermal denaturation principle of protein to prepare the precursor, and further carbonizing the precursor at high temperature in an argon atmosphere to obtain nitrogen-doped porous carbon; the method comprises the following steps:
the method comprises the following steps: pretreatment of egg white: pretreating egg white by a physical dispersion mode to obtain a uniform protein solution;
step two: preparing a precursor solution: adding or not adding a potassium carbonate solution into the protein solution obtained in the step one, stirring and dropwise adding to form a uniform solution, titrating with deionized water, and ultrasonically crushing the liquid by using an ultrasonic cell crusher to obtain a uniform precursor solution;
step three: preparation of the porous carbon precursor: heating the precursor solution obtained in the step two in a water bath at constant temperature to obtain a hydrogel system through protein denaturation gel, and thus obtaining a porous carbon precursor;
step four: drying the porous carbon precursor: freezing the porous carbon precursor obtained in the step three by using liquid nitrogen, and then carrying out freeze drying in a freeze dryer to obtain a dried porous carbon precursor; in the freezing process, the stability of the hydrogel system is kept, no interference such as shaking exists, and the hydrogel system is ensured to be completely frozen; in the freeze drying process, the porous carbon precursor is ensured to be completely dried; for liquid nitrogen freezing, the temperature is-192 ℃, the freezing time is determined according to the amount of the precursor, and the freezing time of different freezing devices is different as long as the freezing is completely ensured: the molds involved in the operation of the present invention take approximately ten minutes to freeze 30ml of precursor in a single pass. For the freeze drying machine, the temperature and the time set by the program of the freeze drying machine with different models can be in and out to a certain extent, as long as the complete drying is ensured: the temperature of the freeze dryer is-60 ℃, and the drying time is 168h (7 days).
Step five, carbonization of the precursor: and heating and carbonizing the dried porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor.
The second embodiment is as follows: in the first step, fresh egg white is separated from eggs, and is subjected to ultrasonic crushing by an ultrasonic cell crusher to obtain a uniform protein (as a main component) solution.
The third concrete implementation mode: in a second specific embodiment, according to the preparation method of the biomass porous carbon electromagnetic wave-absorbing material using egg white as a precursor, the mass fraction of the protein in the protein solution is 10 ± 5 wt% (the mass fractions of the proteins in the protein solutions obtained from different eggs are different).
The fourth concrete implementation mode: in the second specific embodiment, according to the preparation method of the biomass porous carbon electromagnetic wave-absorbing material with egg white as a precursor, the power of ultrasonic crushing is 5-15% of the power of the ultrasonic cell crusher, and the time is 1-2 min.
The fifth concrete implementation mode: in the second step of the preparation method of the biomass porous carbon electromagnetic wave-absorbing material by using egg white as a precursor, the mass concentration of the potassium carbonate solution is 25 wt%; the mass ratio of the potassium carbonate solution to the protein solution obtained in the first step is 0-0.2: 1, preferably 0.1; the requirements of deionized water titration are as follows: the protein solution obtained in the first step accounts for 50 vol% of the precursor solution obtained after titration.
The sixth specific implementation mode: in the second step of the preparation method of the biomass porous carbon electromagnetic wave-absorbing material with egg white as the precursor, the power of ultrasonic crushing is 10-20%, preferably 10%, of the power of the ultrasonic cell crusher, the time is 3-5 min, and the power can be properly reduced to prolong the crushing time.
The seventh embodiment: in the third step, the water bath heating temperature is 80 ℃, and the time is 1-2 hours, preferably 1 hour.
The specific implementation mode is eight: in a specific embodiment, in the fifth step, the carbonization conditions are as follows: pre-carbonizing at 240-320 ℃, wherein the heating rate in the pre-carbonization process is 2 ℃/min, and then carbonizing at 600-800 ℃ for 2h, wherein the preferable carbonization temperature is 700 ℃. The temperature rise rate in the pre-carbonization process refers to a state of keeping the temperature rise in the pre-carbonization process, the temperature rise rate and the pre-carbonization temperature interval are defined, the pre-carbonization time is constant, and the temperature rise rate corresponds to: the pre-carbonization time was 40 min.
Example 1:
a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor is realized according to the following steps:
step one, egg white pretreatment: the method comprises the following steps of pretreating egg white in a physical dispersion mode to obtain a uniform protein solution: separating fresh egg white from eggs, and performing ultrasonic pulverization by using an ultrasonic cell pulverizer to obtain a uniform protein (as a main component) solution, wherein: the mass fraction of the protein in the protein solution is 11.5 wt%; the power of ultrasonic crushing is 5% of the power of the ultrasonic cell crusher, and the crushing time is 1 min;
step two, preparation of precursor solution: adding no potassium carbonate solution, titrating to a certain volume with deionized water, and ultrasonically crushing the liquid with an ultrasonic cell crusher to obtain a uniform precursor solution, wherein: according to the titration requirement, the protein solution obtained in the step one accounts for 50% of the volume fraction of the precursor solution obtained after titration; the crushing power is 10% of the ultrasonic cell crusher power, and the crushing time is 3 min;
step three, preparing a porous carbon precursor: and (3) heating the precursor solution obtained in the step (II) in a water bath kettle in a constant-temperature water bath, and obtaining a hydrogel system through protein denaturation gel, wherein: the temperature of the water bath heating is 80 ℃, and the time is 1 h;
step four, drying the porous carbon precursor: freezing the porous carbon precursor by using liquid nitrogen, and freeze-drying in a freeze dryer to obtain a dried porous carbon precursor, wherein: in the freezing process, the stability of the hydrogel system is kept, no interference such as shaking exists, and the hydrogel system is ensured to be completely frozen; in the freeze drying process, the porous carbon precursor is ensured to be completely dried; for liquid nitrogen freezing, the temperature is-192 ℃, the freezing time is determined according to the amount of the precursor, and the freezing time of different freezing devices is different as long as the freezing is completely ensured: the molds involved in the operation of the present invention take approximately ten minutes to freeze 30ml of precursor in a single pass. For the freeze drying machine, the temperature and the time set by the program of the freeze drying machine with different models can be in and out to a certain extent, as long as the complete drying is ensured: the temperature of the freeze dryer is-60 ℃, and the drying time is 168h (7 days).
Step five, carbonization of the precursor: the method comprises the following steps of heating and carbonizing a dry porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor, wherein: the specific conditions of the carbonization are as follows: heating the mixture from room temperature to 240 ℃ at a speed of 5 ℃/min, heating the mixture from 240 ℃ to 320 ℃ at a speed of 2 ℃/min, heating the mixture to 700 ℃ at a speed of 5 ℃/min, and keeping the temperature for 2 hours to obtain the nitrogen-doped biomass porous carbon electromagnetic wave-absorbing material.
Compared with other electromagnetic wave absorbing materials, the biomass porous carbon electromagnetic wave absorbing material with egg white as the precursor has the characteristics of light weight and high efficiency, when the thickness of the material is only 1.61mm, the maximum absorption peak value at 17.16GHz is 55.9084dB, and when the thickness is 1.79mm, the effective wave absorption width is 5.82GHz, so that the biomass porous carbon electromagnetic wave absorbing material is an excellent electromagnetic wave absorbing material. As shown in fig. 8, it is a micro-topography of the biomass porous carbon obtained in this example. Fig. 6 is a microscopic morphology diagram of the fiber bundle-like structural feature of the biomass porous carbon obtained in this example, and a fine fiber bundle layer can be observed on the surface of the porous carbon.
Example 2:
a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor is realized according to the following steps:
step one, egg white pretreatment: the method comprises the following steps of pretreating egg white in a physical dispersion mode to obtain a uniform protein solution: separating fresh egg white from eggs, and performing ultrasonic pulverization by using an ultrasonic cell pulverizer to obtain a uniform protein (as a main component) solution, wherein: the mass fraction of the protein in the protein solution is 9.5 wt% (the mass fraction of the protein in the protein solution obtained from different eggs can be different); the power of ultrasonic crushing is 10 percent of the power of the ultrasonic cell crusher, and the crushing time is 2 min;
step two, preparation of precursor solution: taking a certain amount of the protein solution obtained in the first step, titrating with deionized water, and ultrasonically crushing the liquid with an ultrasonic cell crusher to obtain a uniform precursor solution, wherein: the mass concentration of the potassium carbonate solution is 25 wt%; the mass ratio of the potassium carbonate solution in the second step to the protein solution obtained in the first step is 0.1: 1; according to the titration requirement, the protein solution obtained in the step one accounts for 50% of the volume fraction of the precursor solution obtained after titration; the crushing power is 10% of the ultrasonic cell crusher power, and the crushing time is 5 min;
step three, preparing a porous carbon precursor: and (3) heating the precursor solution obtained in the step (II) in a water bath kettle in a constant-temperature water bath, and performing protein denaturing gel to obtain a hydrogel system, wherein: the temperature of the water bath heating is 80 ℃, and the time is 1 h;
step four, drying the porous carbon precursor: freezing the porous carbon precursor by using liquid nitrogen, and freeze-drying in a freeze dryer to obtain a dried porous carbon precursor, wherein: in the freezing process, the stability of the hydrogel system is kept, no interference such as shaking exists, and the hydrogel system is ensured to be completely frozen; in the freeze drying process, the porous carbon precursor is ensured to be completely dried; for liquid nitrogen freezing, the temperature is-192 ℃, the freezing time is determined according to the amount of the precursor, and the freezing time of different freezing devices is different as long as the freezing is completely ensured: the molds involved in the operation of the present invention take approximately ten minutes to freeze 30ml of precursor in a single pass. For the freeze drying machine, the temperature and the time set by the program of the freeze drying machine with different models can be in and out to a certain extent, as long as the complete drying is ensured: the temperature of the freeze dryer is-60 ℃, and the drying time is 168h (7 days).
Step five, carbonization of the precursor: the method comprises the following steps of heating and carbonizing a dry porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor, wherein: the specific conditions of the carbonization are as follows: the temperature is raised from room temperature to 240 ℃ at the speed of 5 ℃/min, from 240 ℃ to 320 ℃ at the speed of 2 ℃/min, and then the temperature is raised to the carbonization temperature of 700 ℃ at the speed of 5 ℃/min and kept for 2 hours.
Compared with other electromagnetic wave absorbing materials, the biomass porous carbon electromagnetic wave absorbing material with egg white as a precursor has the characteristics of light weight and high efficiency, when the thickness of the material is only 2.21mm, the maximum wave absorbing peak value at 7.76GHz is 66.15dB, and the effective wave absorbing frequency band width at 1.34mm is 5.09GHz which is higher than the numerical values reported in most documents. As shown in fig. 3, it can be seen that the biomass porous carbon is mainly dielectric loss, and magnetic loss is achieved by electromagnetic matching; as shown in FIG. 5, it can be seen that the biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor has good electromagnetic wave-absorbing performance in the range of 2-18 GHz, and effective wave-absorbing performance can be achieved in the range of 2-18 GHz by adjusting the thickness of the material. Fig. 1 is a schematic diagram of the relationship between the dielectric constant and the frequency of the biomass porous carbon obtained in this example; fig. 2 is a schematic diagram of the relationship between the magnetic permeability and the frequency of the biomass porous carbon obtained in the embodiment; fig. 4 is a schematic diagram of magnetic loss tangent angle of the biomass porous carbon obtained in the embodiment; fig. 9 is a microscopic morphology diagram of the biomass porous carbon obtained in the embodiment.
Example 3:
a preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor is realized according to the following steps:
step one, egg white pretreatment: the method comprises the following steps of pretreating egg white in a physical dispersion mode to obtain a uniform protein solution: separating fresh egg white from eggs, and performing ultrasonic pulverization by using an ultrasonic cell pulverizer to obtain a uniform protein (as a main component) solution, wherein: the mass fraction of the protein in the protein solution is 11 wt% (the mass fraction of the protein in the protein solution obtained from different eggs can be different); the power of ultrasonic crushing is 10 percent of the power of the ultrasonic cell crusher, and the crushing time is 2 min;
step two, preparation of precursor solution: dropwise adding a potassium carbonate solution into the protein solution obtained in the step one while stirring to form a mixed solution, titrating with deionized water, and ultrasonically crushing the liquid by using an ultrasonic cell crusher to obtain a uniform precursor solution, wherein: the mass concentration of the potassium carbonate solution is 25 wt%; the mass ratio of the potassium carbonate solution in the second step to the protein solution obtained in the first step is 0.05: 1; according to the titration requirement, the protein solution obtained in the step one accounts for 50% of the volume fraction of the precursor solution obtained after titration; the crushing power is 10% of the ultrasonic cell crusher power, and the crushing time is 3 min;
step three, preparing a porous carbon precursor: and (3) heating the precursor solution obtained in the step (II) in a water bath kettle in a constant-temperature water bath, and performing protein denaturing gel to obtain a hydrogel system, wherein: the temperature of the water bath heating is 80 ℃, and the time is 1 h;
step four, drying the porous carbon precursor: freezing the porous carbon precursor by using liquid nitrogen, and freeze-drying in a freeze dryer to obtain a dried porous carbon precursor, wherein: in the freezing process, the stability of the hydrogel system is kept, no interference such as shaking exists, and the hydrogel system is ensured to be completely frozen; in the freeze drying process, the porous carbon precursor is ensured to be completely dried; for liquid nitrogen freezing, the temperature is-192 ℃, the freezing time is determined according to the amount of the precursor, and the freezing time of different freezing devices is different as long as the freezing is completely ensured: the molds involved in the operation of the present invention take approximately ten minutes to freeze 30ml of precursor in a single pass. For the freeze drying machine, the temperature and the time set by the program of the freeze drying machine with different models can be in and out to a certain extent, as long as the complete drying is ensured: the temperature of the freeze dryer is-60 ℃, and the drying time is 168h (7 days).
Step five, carbonization of the precursor: the method comprises the following steps of heating and carbonizing a dry porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor, wherein: the specific conditions of the carbonization are as follows: the temperature is raised from room temperature to 240 ℃ at the speed of 5 ℃/min, from 240 ℃ to 320 ℃ at the speed of 2 ℃/min, and then the temperature is raised to the carbonization temperature of 700 ℃ at the speed of 5 ℃/min and kept for 2 hours.
Compared with other electromagnetic wave absorbing materials, the biomass porous carbon electromagnetic wave absorbing material with egg white as a precursor has the characteristics of light weight and high efficiency, and the wave absorbing peak value reaches 55.6687dB at 7.76GHz when the thickness of the material is only 2.21 mm. Fig. 7 is a microscopic morphology diagram of a multi-stage porous structure-like feature of the biomass porous carbon obtained in the present embodiment, where the porous carbon has a composite structure of large pores and small pores, and a groove-shaped texture can still be observed on a pore wall; fig. 10 is a microscopic morphology diagram of the biomass porous carbon obtained in the embodiment, and it can be observed that the introduction of potassium carbonate can obtain a multilevel pore structure with rich content.

Claims (8)

1. A preparation method of a biomass porous carbon electromagnetic wave-absorbing material taking egg white as a precursor is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: pretreatment of egg white: pretreating egg white by a physical dispersion mode to obtain a uniform protein solution;
step two: preparing a precursor solution: adding or not adding a potassium carbonate solution into the protein solution obtained in the step one to form a uniform solution, titrating with deionized water, and ultrasonically crushing the liquid by using an ultrasonic cell crusher to obtain a uniform precursor solution;
step three: preparation of the porous carbon precursor: heating the precursor solution obtained in the second step in a constant-temperature water bath to obtain a porous carbon precursor;
step four: drying the porous carbon precursor: freezing the porous carbon precursor obtained in the step three by using liquid nitrogen, and then carrying out freeze drying in a freeze dryer to obtain a dried porous carbon precursor;
step five, carbonization of the precursor: and heating and carbonizing the dried porous carbon precursor in an argon atmosphere by using a tube furnace to obtain the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor.
2. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 1, characterized by comprising the following steps: in the first step, fresh egg white is separated from eggs, and is subjected to ultrasonic crushing by an ultrasonic cell crusher to obtain a uniform protein solution.
3. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 2, characterized by comprising the following steps: the mass fraction of the protein in the protein solution is 10 +/-5 wt%.
4. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 2, characterized by comprising the following steps: the power of the ultrasonic crushing is 5-15% of that of the ultrasonic cell crusher, and the time is 1-2 min.
5. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 1, characterized by comprising the following steps: in the second step, the mass concentration of the potassium carbonate solution is 25 wt%; the mass ratio of the potassium carbonate solution to the protein solution obtained in the first step is 0-0.2: 1; the requirements of deionized water titration are as follows: the protein solution obtained in the first step accounts for 50 vol% of the precursor solution obtained after titration.
6. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 1, characterized by comprising the following steps: in the second step, the power of the ultrasonic crushing is 10-20% of the power of the ultrasonic cell crusher, and the time is 3-5 min.
7. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 1, characterized by comprising the following steps: in the third step, the water bath heating temperature is 80 ℃, and the time is 1-2 h.
8. The preparation method of the biomass porous carbon electromagnetic wave-absorbing material taking egg white as the precursor according to claim 1, characterized by comprising the following steps: in the fifth step, the concrete conditions of carbonization are as follows: pre-carbonizing at 240-320 ℃, wherein the heating rate in the pre-carbonization process is 2 ℃/min, and then carbonizing for 2h at 600-800 ℃.
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* Cited by examiner, † Cited by third party
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CN111151283B (en) * 2020-01-15 2021-04-20 中南大学 Nitrogen-cobalt co-doped porous carbon loaded sulfur-zinc-cobalt catalytic material and preparation method and application thereof
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106517157A (en) * 2016-10-28 2017-03-22 华北电力大学 Nitrogen-doped carbon nanofiber/graphene aerogel preparation method and application
CN108615899A (en) * 2018-04-27 2018-10-02 中南大学 A kind of Heteroatom doping porous carbon materials and preparation method thereof and the application in zinc and air cell
CN109336106A (en) * 2018-10-29 2019-02-15 宿州学院 A kind of preparation method of bean dregs base nitrogen boron codope porous carbon materials

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002020994A (en) * 2000-07-05 2002-01-23 Tomoji Tanaka Electromagnetic wave absorbing material and processed article applying the same
CN103979530A (en) * 2014-06-11 2014-08-13 安徽工业大学 Method for preparing porous carbon for electrochemical capacitor from egg white used as raw material
CN104843668A (en) * 2015-04-23 2015-08-19 北京理工大学 Method for preparing nitrogen doped porous carbon material by using biologic proteins
CN108199150A (en) * 2017-12-30 2018-06-22 吴迪 A kind of preparation method of the carbon-based absorbing material of strong absorbent
CN109666451B (en) * 2019-01-21 2021-08-24 淮北师范大学 Method for preparing wave-absorbing material by using biomass carbon source
CN109879270B (en) * 2019-04-24 2022-02-08 哈尔滨工业大学 Preparation method of light ultra-wideband carbonized waxberry wave-absorbing material
CN110079271B (en) * 2019-05-15 2020-03-10 吉林大学 Protein-based carbon/magnetic Fe Co nanoparticle composite wave absorber and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106517157A (en) * 2016-10-28 2017-03-22 华北电力大学 Nitrogen-doped carbon nanofiber/graphene aerogel preparation method and application
CN108615899A (en) * 2018-04-27 2018-10-02 中南大学 A kind of Heteroatom doping porous carbon materials and preparation method thereof and the application in zinc and air cell
CN109336106A (en) * 2018-10-29 2019-02-15 宿州学院 A kind of preparation method of bean dregs base nitrogen boron codope porous carbon materials

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