CN115386337A - Chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and preparation method thereof - Google Patents
Chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and a preparation method thereof. The preparation method provided by the invention has the advantages of simple synthesis process, abundant material resources, environment friendliness and wide application prospect, and the prepared chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is used for electromagnetic wave absorption and has excellent performance.
Description
Technical Field
The invention relates to the technical field of nano composite materials and electromagnetic wave absorption, in particular to a chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and a preparation method thereof.
Background
Based on the high-speed development and the wide application of information technology, electromagnetic radiation pollution becomes fourth environmental pollution following water, air and noise, the problem of electromagnetic pollution seriously threatens human health and information safety, and the electromagnetic pollution becomes one of the important problems to be solved urgently in the development of the current society. Electromagnetic absorption is the most effective method for really solving the electromagnetic radiation pollution, and the research and development of a high-performance electromagnetic wave absorbent with the characteristics of thinness, lightness, width and strength is urgent. The wave-absorbing material in the prior art has the problems of large density, narrow wave-absorbing frequency band, complex synthesis process, expensive raw materials, single loss mechanism and the like.
Compared with the traditional polyaniline, the chiral polyaniline can show special optical rotation and circular dichroism due to the unique supercoiled structure, and generates a cross polarization coupling effect under the action of an alternating electromagnetic field, so that the chiral polyaniline has a multiple electromagnetic wave loss mechanism, is low in sensitivity to frequency, can effectively widen an absorption frequency band, and is one of conductive polymers with application prospects.
Carbon black, graphene, carbon fiber, carbon nanotube and the like are important carbon-based wave-absorbing materials, but the preparation cost is high, the energy consumption is large, and the industrial application scale is restricted. Therefore, the method is very important for searching green, environment-friendly, low-price and high-efficiency carbon materials. The biomass-derived porous carbon is a new carbon material, has the advantages of rich resources, environmental protection, low price, excellent electric conduction, adjustable pore channel structure, large specific surface area and the like, and is a candidate for synthesizing a carbon-based composite wave-absorbing material with great potential value. The pore structure can effectively regulate and control dielectric constant, optimize impedance matching, simultaneously enable incident electromagnetic waves to generate multiple reflection and scattering, extend the propagation path of the electromagnetic waves and provide more opportunities for absorbing and attenuating electromagnetic wave energy. The high specific surface area of the chiral polyaniline provides rich sites for the growth of chiral polyaniline, and contributes to the construction of a heterogeneous interface and the improvement of interface polarization. Therefore, optimization of microstructure and material composition is a potential approach to address the growing problem of electromagnetic interference.
Chinese patent CN201210005404.0 discloses an expanded graphite/polyaniline/cobalt ferrite wave-absorbing material and a preparation process thereof, wherein the preparation process comprises the following steps: preparing expanded graphite; (2) preparing absolute ethyl alcohol containing expanded graphite; (3) preparing an expanded graphite/polyaniline binary compound; (4) Preparing an expanded graphite/polyaniline/cobalt ferrite ternary compound; (5) Weighing the expanded graphite/polyaniline/cobalt ferrite ternary complex and paraffin, uniformly mixing, and performing ball milling to obtain the expanded graphite/polyaniline/cobalt ferrite wave-absorbing material. The polyaniline wave-absorbing material has moderate capability of absorbing electromagnetic waves through a dual mechanism of dielectric loss and magnetic loss, and has poor overall performance.
Chinese patent CN201210034964.9 discloses a preparation method of a neodymium-doped manganese-zinc ferrite-polyaniline composite wave-absorbing material, wherein neodymium-doped manganese-zinc ferrite with different doping amounts is prepared by a chemical codeposition method according to the stoichiometric proportion of Mn0.4Zn0.6NdxFe2-xO4 (x = 0.025-0.1); and then preparing (5-20%) neodymium-doped manganese-zinc ferrite-polyaniline composite wave-absorbing material by an in-situ compounding method according to the mass ratio of the neodymium-doped manganese-zinc ferrite to the aniline monomer of 1-4. The preparation process is complex, the preparation time is long, and the production cost for preparing the polyaniline wave-absorbing material is high.
Disclosure of Invention
The invention aims to provide a chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and a preparation method thereof. The prepared chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is used for electromagnetic wave absorption and has excellent performance.
In order to solve the technical problems, the invention adopts a specific scheme that a preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material comprises the following steps: the biomass material is carbonized at high temperature to prepare biomass-derived porous carbon, and under the combined action of a chiral compound inducer and an initiator, chiral polyaniline is polymerized on the surface of the biomass-derived porous carbon to prepare the composite wave-absorbing material.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: the method specifically comprises the following steps:
s1: removing impurities from a biomass material, crushing, immersing the biomass material in a KOH solution, filtering and drying to obtain biomass powder for later use;
s2: calcining the biomass powder obtained in the step S1 in an inert atmosphere, naturally cooling to room temperature after the calcination is finished, grinding, washing, and freeze-drying to obtain biomass-derived porous carbon powder for later use;
s3: immersing the biomass-derived porous carbon powder prepared in the step S2 into an aniline monomer and chiral compound inducer aqueous solution to prepare suspension pre-solution, and cooling to 0-5 ℃;
s4: and (3) dissolving an initiator in deionized water, then dropwise adding the initiator into the suspension pre-solution prepared in the step (S3), and filtering, washing, centrifuging and freeze-drying to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: the biomass material in the step S1 refers to crop straws or shell waste, wherein the crop straws are straws of corn, sorghum, sunflower or wheat, and the shell waste is shells of peanuts, walnuts or nuts.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: and in the step S1, the biomass material is crushed and then sieved by a 20-300-mesh sieve, the concentration of KOH solution is 0.5-3mol/L, and the biomass material is immersed in the KOH solution, then is subjected to ultrasonic oscillation for 10-30min and then is kept stand for 3-12h.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: and in the step S2, the biomass powder is calcined in a tubular furnace, the temperature rise rate in the calcining process is 2-15 ℃/min, the calcining temperature is 500-800 ℃, and the heat preservation time is 1-5h.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: the chiral compound inducer consists of a chiral compound inducer main body and a compound additive, wherein the mass ratio of the inducer main body to the compound additive is (10-10).
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: in the step S3, the mass ratio of the aniline monomer to the chiral compound inducer is 1:1-1:4.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: in the step S4, the initiator is ammonium persulfate, ferric trichloride, potassium permanganate or hydrogen peroxide, and the mass ratio of the initiator to the aniline monomer in the suspension pre-solution is 1:1-1.
The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material is further optimized as follows: in the step S4, the acceleration of the drop of the initiator aqueous solution is 1-10ml/min, the dropping is carried out at the stirring speed of 50-300r/min, and the still standing reaction is carried out for 10-24h after the dropping is finished.
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material is prepared by any one of the preparation methods.
Advantageous effects
According to the preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material, the biomass-derived porous carbon prepared by high-temperature carbonization and activation is used as a substrate, and the adjustable unique pore structure, the high specific surface and a large number of surface functional groups provide sufficient attachment and growth sites for the chiral polyaniline. Under the unique induction of the chiral compound inducer, the polyaniline and the initiator have synergistic effect, the polyaniline main chain preferentially adopts a spiral configuration to obtain chiral polyaniline and is attached to the surface of the biomass-derived porous carbon to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material. The chiral polyaniline can show special optical rotation and circular dichroism due to a unique supercoiled structure, and a cross polarization coupling effect is generated under the action of an alternating electromagnetic field, so that the chiral polyaniline has a multiple electromagnetic wave loss mechanism, the absorption performance can be effectively regulated and controlled by regulating chiral parameters, impedance matching is easier to realize than regulating electromagnetic parameters, and meanwhile, based on a biomass-derived porous carbon substrate, the chiral composite material has a unique three-dimensional pore channel structure, which is beneficial to establishing a three-dimensional conductive network, prolonging an electromagnetic wave transmission channel, enhancing multiple reflection and scattering, and further showing excellent electromagnetic wave absorption and attenuation characteristics. The method has the advantages of simple synthesis process, abundant material resources, environmental friendliness and wide application prospect.
Drawings
FIG. 1 is an SEM image of a composite wave-absorbing material prepared in example 1;
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to specific embodiments, but the scope of the present invention is not limited to the embodiments, and modifications made to the technical solutions of the present invention by those skilled in the art should fall within the scope of the present invention.
Example 1
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) Repeatedly cleaning peanut shells to remove surface impurities, drying, crushing, sieving with a 50-mesh sieve, then immersing in a KOH solution with the concentration of 1mol/L, standing for 12h after ultrasonic oscillation for 30min, and then filtering and drying.
2) The prepared biomass powder is put into a tube furnace in N 2 Calcining under the protection of atmosphere, wherein the heating rate is 5 ℃/min, the calcining temperature is 750 ℃, the heat preservation time is 2h, naturally cooling to room temperature, grinding, pickling with hydrochloric acid, washing with water for multiple times, and freeze-drying to obtain the biomass-derived porous carbon powder.
3) Fully dissolving 0.5ml of aniline monomer, 1.16g of camphorsulfonic acid and 0.17g of mandelic acid in 50ml of deionized water, weighing 0.5g of biomass-derived porous carbon powder, immersing the biomass-derived porous carbon powder in the solution, performing ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, and cooling the suspension pre-solution to 0-5 ℃ in an ice water bath.
4) Weighing 1.25g of ammonium persulfate, sufficiently dissolving in 20ml of deionized water, cooling to a constant temperature in an ice water bath, dropwise adding into the suspension of aniline monomer, camphorsulfonic acid, mandelic acid and biomass-derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, slowly stirring at 100r/min in the dropwise adding process, stopping stirring after the dropwise adding is finished, standing in the ice water bath for 24 hours for reaction, and filtering, washing, centrifuging and freeze-drying to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material (the SEM image of the wave-absorbing material is shown in figure 1).
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the wave-absorbing performance of the polyaniline/biomass-derived porous carbon composite material at the frequency of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 1.8mm, the minimum reflection loss value can reach-42.58 dB, and the effective absorption bandwidth can reach 4.5GHz.
Example 2
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) The walnut shells are repeatedly cleaned to remove surface impurities, dried, crushed, sieved by a 20-mesh screen, then immersed in 2mol/L KOH solution, subjected to ultrasonic oscillation for 30min, kept stand for 8h, filtered and dried.
2) The biomass powder obtained is placed in a tube furnace in N 2 Calcining under the protection of atmosphere, wherein the heating rate is 5 ℃/min, the calcining temperature is 800 ℃, the heat preservation time is 3h, naturally cooling to room temperature, grinding, pickling with hydrochloric acid, washing with water, and freeze-drying to obtain the biomass-derived porous carbon powder.
3) Fully dissolving 0.4ml of aniline monomer, 1g of camphorsulfonic acid, 0.05g of mandelic acid and 0.25g of p-methyl dibenzoyl tartaric acid in 30ml of deionized water, weighing 0.4g of biomass-derived porous carbon powder, immersing the biomass-derived porous carbon powder in the solution, performing ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, and cooling the suspension pre-solution to 0-5 ℃ in an ice water bath.
4) Weighing 0.8g of ferric trichloride, fully dissolving the ferric trichloride in 15ml of deionized water, cooling the mixture in an ice-water bath to a constant temperature, dropwise adding the mixture into a suspension of aniline monomer, camphorsulfonic acid, mandelic acid, p-toluyl tartaric acid and biomass-derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, stirring the mixture at a slow speed of 80r/min in the dropwise adding process, stopping stirring the mixture after the dropwise adding is finished, standing the mixture in the ice-water bath for reacting for 24 hours, and filtering, washing, centrifuging and freeze-drying the mixture to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the wave-absorbing performance of the polyaniline/biomass-derived porous carbon composite material at the frequency of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 2.1mm, the minimum reflection loss value can reach-39.64 dB, and the effective absorption bandwidth can reach 4.32GHz.
Example 3
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) Repeatedly cleaning sorghum straws to remove surface impurities, drying, crushing, sieving with a 20-mesh sieve, then soaking in a KOH solution with the concentration of 1.5mol/L, standing for 8 hours after ultrasonic oscillation for 30min, and then filtering and drying.
2) The prepared biomass powder is put into a tube furnace in N 2 Calcining under the atmosphere protection, wherein the heating rate is 5 ℃/min, the calcining temperature is 750 ℃ and the heat preservation time is 1h in the calcining process, naturally cooling to the room temperature, grinding, washing with hydrochloric acid and water, and freeze-drying to obtain the biomass-derived porous carbon powder.
3) Fully dissolving 0.5ml aniline monomer, 1.2g camphorsulfonic acid, 0.3g p-methyl dibenzoyl tartaric acid and 0.01ml chloropropionic acid in 30ml deionized water, weighing 0.5g biomass-derived porous carbon powder, immersing the biomass-derived porous carbon powder in the solution, performing ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, and cooling the suspension pre-solution to 0-5 ℃ in an ice water bath.
4) Weighing 1.2g of ammonium persulfate, sufficiently dissolving in deionized water, cooling in an ice-water bath to a constant temperature, then dropwise adding into a suspension of aniline monomer, camphorsulfonic acid, p-toluyl tartaric acid, chloropropionic acid and biomass-derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, slowly stirring at 150r/min in the dropwise adding process, stopping stirring after the dropwise adding is finished, placing in the ice-water bath, standing for reacting for 24 hours, and then filtering, washing, centrifuging and freeze-drying to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the polyaniline/biomass-derived porous carbon composite material under the wave-absorbing performance of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 2.4mm, the minimum reflection loss value can reach-40.54 dB, and the effective absorption bandwidth can reach 4.28GHz.
Example 4
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) Cleaning sunflower straws repeatedly to remove surface impurities, drying, crushing, sieving with a 80-mesh sieve, immersing in a KOH solution with the concentration of 1.5mol/L, ultrasonically oscillating for 30min, standing for 12h, filtering and drying.
The prepared biomass powder is put into a tube furnace in N 2 Calcining under the protection of atmosphere, wherein the heating rate is 5 ℃/min, the calcining temperature is 750 ℃, the heat preservation time is 2h, naturally cooling to room temperature, grinding, pickling with hydrochloric acid, washing with water, and freeze-drying to obtain the biomass-derived porous carbon powder.
2) Fully dissolving 0.45ml aniline monomer, 1.1g camphorsulfonic acid, 0.25g p-methyl dibenzoyl tartaric acid and 0.01ml chloropropionic acid in 30ml deionized water, weighing 0.4g biomass derived porous carbon powder, immersing the solution in the solution, performing ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, and cooling to 0-5 ℃ in an ice water bath.
3) Weighing 0.75g of ferric trichloride, fully dissolving the ferric trichloride in deionized water, cooling the mixture in an ice-water bath to a constant temperature, dropwise adding the mixture into a suspension of aniline monomer, camphorsulfonic acid, p-toluyl tartaric acid, chloropropionic acid and biomass-derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, stirring the mixture at a slow speed of 100r/min in the dropwise adding process, stopping stirring the mixture after the dropwise adding is finished, standing the mixture in the ice-water bath for reaction for 24 hours, and filtering, washing, centrifuging and freeze-drying the mixture to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the wave-absorbing performance of the polyaniline/biomass-derived porous carbon composite material at the frequency of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 2mm, the minimum reflection loss value can reach-41.92 dB, and the effective absorption bandwidth can reach 4.06GHz.
Comparative example 1
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) Repeatedly cleaning peanut shells to remove surface impurities, drying, crushing, sieving with a 50-mesh sieve, then immersing in a KOH solution with the concentration of 1mol/L, standing for 12h after ultrasonic oscillation for 30min, and then filtering and drying.
2) The prepared biomass powder is put into a tube furnace in N 2 Calcining under the protection of atmosphere, wherein the heating rate is 5 ℃/min, the calcining temperature is 750 ℃, the heat preservation time is 2h, naturally cooling to room temperature, grinding, pickling with hydrochloric acid, washing with water for multiple times, and freeze-drying to obtain the biomass-derived porous carbon powder.
3) Fully dissolving 0.5ml of aniline monomer into 50ml of deionized water, weighing 0.5g of biomass-derived porous carbon powder, immersing the biomass-derived porous carbon powder into the solution, performing ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, and cooling the suspension pre-solution to 0-5 ℃ in an ice water bath.
4) Weighing 1.25g of ammonium persulfate, sufficiently dissolving the ammonium persulfate in 20ml of deionized water, cooling the mixture to a constant temperature in an ice water bath, dropwise adding the mixture into the suspension of aniline monomer and biomass-derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, slowly stirring the mixture at a speed of 100r/min in the dropwise adding process, stopping stirring after the dropwise adding is finished, placing the mixture in the ice water bath, standing the mixture for reaction for 24 hours, and then filtering, washing, centrifuging and freeze-drying the mixture to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the wave-absorbing performance of the polyaniline/biomass-derived porous carbon composite material at the frequency of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 1.6mm, the minimum reflection loss value can reach-21.36 dB, and the effective absorption bandwidth can reach 2.88GHz.
Comparative example 2
A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and a preparation method thereof comprise the following steps:
1) Repeatedly cleaning peanut shells to remove surface impurities, drying, crushing, sieving with a 50-mesh sieve, then immersing in a KOH solution with the concentration of 1mol/L, standing for 12h after ultrasonic oscillation for 30min, and then filtering and drying.
2) The prepared biomass powder is put into a tube furnace in N 2 Calcining under the protection of atmosphere, wherein the heating rate is 5 ℃/min, the calcining temperature is 750 ℃, the heat preservation time is 2h, naturally cooling to room temperature, grinding, pickling with hydrochloric acid, washing with water for multiple times, and freeze-drying to obtain the biomass-derived porous carbon powder.
3) 0.5ml of aniline monomer and 1.16g of camphorsulfonic acid are fully dissolved in 50ml of deionized water to prepare the solution, 0.5g of biomass-derived porous carbon powder is weighed and immersed in the solution, and after the solution is subjected to ultrasonic treatment and stirring to obtain uniform and stable suspension pre-solution, the solution is cooled to 0-5 ℃ in an ice water bath.
4) Weighing 1.25g of ammonium persulfate, fully dissolving the ammonium persulfate in 20ml of deionized water, cooling the mixture to a constant temperature in an ice water bath, dropwise adding the mixture into the suspension of aniline monomer, camphorsulfonic acid and biomass derived porous carbon powder at a constant speed of 3ml/min through a constant-pressure dropping funnel, slowly stirring the mixture at a speed of 100r/min in the dropwise adding process, stopping stirring the mixture after the dropwise adding is finished, placing the mixture in the ice water bath, standing the mixture for reaction for 24 hours, and filtering, washing, centrifuging and freeze-drying the mixture to obtain the chiral polyaniline/biomass derived porous carbon composite wave-absorbing material.
Wave-absorbing property: based on a coaxial reflection/transmission method, a vector network analyzer is adopted to test the wave-absorbing performance of the polyaniline/biomass-derived porous carbon composite material at the frequency of 2-18 GHz. The sample size was: 7.00mm of outer diameter, 3.00mm of inner diameter and 2.00mm of thickness. The paraffin matrix and the polyaniline/biomass derived porous carbon composite wave-absorbing material are uniformly mixed according to the mass ratio of 4:1, and then pressed into a coaxial circular ring by using a specific mould for testing. When the thickness of the material is 1.7mm, the minimum reflection loss value can reach-33.68 dB, and the effective absorption bandwidth can reach 3.8GHz.
According to the comparative example 1, the wave-absorbing performance of the finally prepared material is obviously reduced without adding the composite inducer in the preparation process of the wave-absorbing material, and according to the comparative example 2, only the inducer main body is added and no additive is added in the preparation process of the wave-absorbing material, so that the wave-absorbing performance of the finally prepared material is obviously improved but still lower than that of the materials in the examples 1-4. It can be seen from this that: under the unique induction of the chiral compound inducer, the polyaniline and the initiator have synergistic effect, the polyaniline main chain preferentially adopts a spiral configuration to obtain chiral polyaniline and is attached to the surface of the biomass-derived porous carbon to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material. The chiral polyaniline can show special optical rotation and circular dichroism due to a unique supercoiled structure, and a cross polarization coupling effect is generated under the action of an alternating electromagnetic field, so that the chiral polyaniline has a multiple electromagnetic wave loss mechanism, the absorption performance can be effectively regulated and controlled by regulating chiral parameters, and compared with the regulation of electromagnetic parameters, the impedance matching is easier to realize.
Claims (10)
1. A preparation method of a chiral polyaniline/biomass derived porous carbon composite wave-absorbing material is characterized by comprising the following steps: the biomass material is carbonized at high temperature to prepare biomass-derived porous carbon, and under the combined action of a chiral compound inducer and an initiator, chiral polyaniline is polymerized on the surface of the biomass-derived porous carbon to prepare the composite wave-absorbing material.
2. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 1, which is characterized by comprising the following steps: the method specifically comprises the following steps:
s1: removing impurities from a biomass material, crushing, immersing the biomass material in a KOH solution, filtering and drying to obtain biomass powder for later use;
s2: calcining the biomass powder obtained in the step S1 in an inert atmosphere, naturally cooling to room temperature after the calcination is finished, grinding, washing, and freeze-drying to obtain biomass-derived porous carbon powder for later use;
s3: immersing the biomass-derived porous carbon powder prepared in the step S2 into an aniline monomer and chiral compound inducer aqueous solution to prepare suspension pre-solution, and cooling to 0-5 ℃;
s4: and (3) dissolving an initiator in deionized water, then dropwise adding the initiator into the suspension pre-solution prepared in the step (S3), and filtering, washing, centrifuging and freeze-drying to obtain the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material.
3. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: the biomass material in the step S1 refers to crop straws or shell waste, wherein the crop straws are straws of corn, sorghum, sunflower or wheat, and the shell waste is shells of peanuts, walnuts or nuts.
4. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: and in the step S1, the biomass material is crushed and then passes through a 20-300-mesh sieve, the concentration of the KOH solution is 0.5-3mol/L, the biomass material is immersed in the KOH solution and then is subjected to ultrasonic oscillation for 10-30min, and then the biomass material is kept stand for 3-12h.
5. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: and in the step S2, the biomass powder is calcined in a tubular furnace, the temperature rise rate in the calcining process is 2-15 ℃/min, the calcining temperature is 500-800 ℃, and the heat preservation time is 1-5h.
6. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: the chiral compound inducer consists of a chiral compound inducer main body and a compound additive, the mass ratio of the inducer main body to the compound additive is 10-10.
7. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: in the step S3, the mass ratio of the aniline monomer to the chiral compound inducer is 1:1-1:4.
8. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: in the step S4, the initiator is ammonium persulfate, ferric trichloride, potassium permanganate or hydrogen peroxide, and the mass ratio of the initiator to the aniline monomer in the suspension pad fluid is 1:1-1.
9. The preparation method of the chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material according to claim 2, which is characterized by comprising the following steps: in the step S4, the acceleration of the drop of the initiator aqueous solution is 1-10ml/min, the dropping is carried out at the stirring speed of 50-300r/min, and the still standing reaction is carried out for 10-24h after the dropping is finished.
10. A chiral polyaniline/biomass derived porous carbon composite wave-absorbing material is characterized in that: prepared by the preparation method of any one of claims 1 to 9.
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