Multi-province and quinone-based composite nano wave-absorbing material and preparation method thereof
By preparing a composite nanomaterial of multi-quinone polymer loaded with magnetic nanoparticles, the problem of insufficient weather resistance and environmental adaptability of existing absorbing materials under extreme conditions has been solved, achieving high-efficiency absorbing performance over a wide frequency band. This material is suitable for weapon stealth technology and the solution of electromagnetic radiation pollution.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-21
- Publication Date
- 2026-03-31
AI Technical Summary
Existing radar-absorbing materials have shortcomings in terms of thinness, light weight, wide absorption frequency band, and strong absorption capacity. Furthermore, they lack weather resistance and environmental adaptability under extreme conditions, making it difficult to meet the requirements of weapon stealth technology and electromagnetic radiation pollution.
Using polyquinone polymers as the matrix, polyquinone polymers are prepared by solid-state reaction method, and magnetic nanoparticles such as iron(III) oxide are loaded by hydrothermal method to form composite nano-absorbing materials. The dielectric loss is improved by utilizing the molecular mobility polarization characteristics and dielectric relaxation behavior, and the impedance matching characteristics are improved.
It achieves a reflection loss of less than -10dB in the frequency range of 13.2-17.9GHz, and a maximum absorption intensity of -46.6dB when the thickness is 1.50mm. It has wide absorption and strong absorption performance, and the material has low density, corrosion resistance and good thermal stability, making it suitable for widespread application.
Smart Images

Figure CN116948384B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of microwave absorbing materials technology, specifically relating to a composite nano-absorbing material based on multi-quinone polymers and its preparation method. Background Technology
[0002] With the in-depth development of precision-guided weapons, stealth technology has become a key research focus in the defense and military field. Meanwhile, the widespread use of electronic products and wireless communication technologies has made electromagnetic pollution another major problem after air pollution, water pollution, and light pollution. Absorbing materials are a key solution for developing weapon stealth technology and addressing electromagnetic radiation pollution. Absorbing materials are materials that can absorb the energy of electromagnetic waves incident on their surface, thereby reducing electromagnetic interference or concealing electromagnetic signals. To better achieve the goals of electronic equipment integration or lightweight aerospace weapons, absorbing materials should typically meet performance requirements such as thinness, light weight, wide absorption frequency band, and strong absorption capacity. They should also possess stable temperature resistance, corrosion resistance, and good multi-band compatibility.
[0003] Microwave absorbing materials typically utilize carbon materials, ferromagnetic metals, and ferrites. However, these materials are often limited by their inherent susceptibility to oxidation, high density, and limited loss mechanisms. Furthermore, applications under extreme conditions require microwave absorbing materials with good weather resistance and environmental adaptability. Polymers, on the other hand, are characterized by low density, light weight, and ease of processing. They also possess unique advantages in terms of temperature resistance, oxidation resistance, and corrosion resistance. Polymers such as polyaniline, polypyrrole, and polythiophene exhibit certain conductivity due to the delocalization of π electrons. By controlling the structure, morphology, and doping type, microwave absorbing properties can be achieved. For example, polypyrrole with a helical conductive network prepared by chiral induction exhibits microwave absorbing properties in the 8.0-11.5 GHz range (J. Mater. Chem. C, 2017, 5, 2175-2181).
[0004] From the perspective of energy loss, improving microwave absorption performance can be achieved by optimizing the composition and structure of the dielectric material, utilizing strong dielectric loss to obtain strong and wide absorption effects. Simultaneously, based on impedance matching, the overall loss capacity of the material can be maximized. Composite microwave absorbing materials composed of magnetic and dielectric materials represent an important development direction. This not only allows for improved impedance matching through material composition control but also leverages the synergistic mechanism of magnetic and dielectric losses based on multiple components. Therefore, developing a composite microwave absorbing material composed of magnetic and dielectric materials is of great significance for developing weapon stealth technology and addressing electromagnetic radiation pollution problems. Summary of the Invention
[0005] This invention provides a composite nanomaterial based on polyquinone polymers (PAQR) and its preparation method. PAQR utilizes molecular mobility polarization and dielectric relaxation behavior to achieve significant dielectric loss. Loading nanomagnetic particles such as iron(III) oxide (Fe3O4) can improve the electromagnetic properties of PAQR, thereby enhancing the overall loss capability of the material system and improving impedance matching characteristics, thus facilitating better microwave absorption performance. Furthermore, iron(III) oxide and similar materials are inexpensive and readily available, making them suitable for widespread application.
[0006] The technical solution of this invention is as follows:
[0007] In the first aspect, a method for preparing composite nano-absorbing materials based on multi-quinone polymers is disclosed, including the following steps:
[0008] 1) Preparation of polyquinone polymers by solid-state reaction method: Anthraquinone and pyromellitic anhydride were used as reactants and Lewis acid was used as catalyst. After being mixed evenly, the mixture was calcined in an inert atmosphere, purified, dried and thoroughly ground to obtain polyquinone polymers.
[0009] 2) Using the polyquinone polymer prepared in step 1) as the matrix material, the loading of nanomagnetic particles on the surface of the polymer was achieved by hydrothermal method: ferromagnetic metal salt was dissolved in a solvent, polyethylene glycol 1000 monomethyl ether and sodium acetate were added, and the mixture was stirred to form a uniform solution. The polyquinone polymer powder obtained in step 1) was placed in the above solution, ultrasonically dispersed uniformly, subjected to hydrothermal reaction, centrifuged, and dried to obtain a composite nano-absorbing material based on the polyquinone polymer.
[0010] Preferably, the molar ratio of anthraquinone, pyromellitic anhydride, and Lewis acid is 1:1:1-2.
[0011] Preferably, the Lewis acid is one of zinc chloride or aluminum chloride.
[0012] Preferably, in step 1), the calcination is carried out at 300-330°C in an inert atmosphere for 6-24 hours.
[0013] Preferably, the inert atmosphere in step 1) is either nitrogen or argon.
[0014] Preferably, in step 1), the purification is carried out by extracting the sample in a Soxhlet extractor with 10% hydrochloric acid solution, deionized water, anhydrous ethanol and toluene for 12-24 hours each, and the drying is carried out by vacuum drying at 60-80°C.
[0015] Preferably, step 2) involves dissolving 0.2-1.0 g of a ferromagnetic metal salt in 20-100 mL of solvent, adding 0.2-1.0 g of polyethylene glycol 1000 monomethyl ether and 0.6-1.5 g of sodium acetate, and stirring on a magnetic stirrer to form a homogeneous solution. Then, 0.1-2.0 g of the polyquinone polymer powder obtained in step 1) is placed in the above solution and sonicated for 0.5 h to ensure thorough dispersion. The solution is then transferred to a hydrothermal reactor, and the hydrothermal reaction temperature is 150-220 °C for 4-24 h. After centrifugation, the resulting reaction product is washed with deionized water and anhydrous ethanol, and finally vacuum dried at 60 °C to obtain a composite nano-absorbing material based on polyquinone polymers.
[0016] Preferably, the solvent is one of deionized water, ethylene glycol, ethanol, etc.
[0017] Preferably, the ferromagnetic metal salt is one of ferric chloride, ferric nitrate, ferric sulfate, cobalt chloride, cobalt nitrate, nickel chloride, nickel nitrate, etc., and their hydrated salts.
[0018] Secondly, a method for preparing the composite nano-absorbing material based on multi-quinone polymers is provided, which yields the composite nano-absorbing material based on multi-quinone polymers.
[0019] Polyquinone polymers are planar conjugated polymers with semiconductor properties, formed by aromatic rings or heterocyclic compounds and acid anhydrides. Compared to carbon materials, ferromagnetic metals, and ferrites, they exhibit lower density, corrosion resistance, and better thermal stability. Furthermore, polyquinone polymers possess a large molecular conjugated structure, allowing internal charge carriers to form extremely large molecular dipole moments. This unique mobile polarization and large polarization shift result in a significant relaxation behavior of the dielectric constant with increasing frequency, leading to substantial dielectric loss. This is a significant characteristic that distinguishes these polymers from other polymer materials, making them suitable as high-dielectric-loss absorbing materials. The unique molecular mobile polarization characteristics of polyquinone polymers, completely different from other polymer materials, show promising application prospects in electromagnetic attenuation and microwave absorption. Utilizing these molecular mobile polarization characteristics and their dielectric relaxation behavior can yield significant dielectric loss, facilitating the design and fabrication of polymer microwave absorbing materials. Loading nano-magnetic particles such as iron oxide can improve the electromagnetic properties of polyquinone polymers. On the one hand, it can improve the overall loss capacity of the material system, and on the other hand, it can improve the impedance matching characteristics, which is conducive to achieving better wave absorption performance. At the same time, iron oxide and other materials are inexpensive and readily available, making them suitable for widespread application.
[0020] Compared with the prior art, the present invention has the following advantages:
[0021] 1. The composite nano-absorbing material based on polyquinone polymers of the present invention uses polyquinone polymers as the matrix and selects ferromagnetic nanoparticles to modify the polymer matrix. The absorbing material achieves a reflection loss of less than -10dB in the frequency range of 13.2-17.9GHz, that is, it can absorb 90% of the incident electromagnetic waves in a frequency band of 4.7GHz.
[0022] 2. The composite nano-absorbing material based on multi-quinone polymers prepared in this invention achieves a maximum absorption intensity of -46.6dB at 15.0GHz when the thickness is 1.50mm. As the thickness is changed, the effective absorption bandwidth and intensity of the prepared composite nano-absorbing material based on multi-quinone polymers also change accordingly. This allows for effective control of the absorption performance and achieves the performance goals of wide absorption and strong absorption.
[0023] 3. This invention is the first to achieve the modification of multi-agent quinone polymers by nanomagnetic particles through a hydrothermal method, preparing a composite nanomaterial based on multi-agent quinone polymers, which exhibits high-efficiency microwave absorption performance. This invention has the advantages of novel materials, simple preparation process, good repeatability, and mass production capability, making the nanomagnetic particle-modified multi-agent quinone polymer composite material have a good application prospect in the field of microwave absorption materials. Attached Figure Description
[0024] Figure 1 The X-ray diffraction pattern of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1 is shown below.
[0025] Figure 2 The image shows a scanning electron microscope (SEM) image of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1.
[0026] Figure 3 The hysteresis loop of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1;
[0027] Figure 4 The reflection loss of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1 is shown.
[0028] Figure 5 The reflection loss of the composite nano-absorbing materials based on polyquinone polymers prepared in Examples 5-7 and Comparative Example 1 is shown. Detailed Implementation
[0029] Example 1
[0030] The preparation method of the composite nano-absorbing material based on multi-quinone polymers is as follows:
[0031] 1) Preparation of polyquinone polymers by solid-phase reaction method: Anthraquinone, pyromellitic anhydride and zinc chloride were weighed in a molar ratio of 1:1:1 and thoroughly ground in an agate mortar to make them evenly mixed. The mixture was poured into a porcelain boat and placed in a tube furnace. It was heated to 300℃ in a nitrogen atmosphere and kept at that temperature for 6 hours. After being taken out, it was ground and purified by Soxhlet extraction with 10% hydrochloric acid solution, deionized water, anhydrous ethanol and toluene for 12 hours each. Finally, it was vacuum dried at 60℃ and thoroughly ground to obtain polyquinone polymer powder.
[0032] 2) Dissolve 0.53g of ferric chloride in 40mL of ethylene glycol, add 0.53g of polyethylene glycol 1000 monomethyl ether and 1.44g of sodium acetate, and stir on a magnetic stirrer to form a homogeneous solution. Then, add 0.4g of the polyquinone polymer powder obtained in step 1) to the above solution and sonicate for 0.5h to ensure thorough dispersion. Transfer the solution to a hydrothermal reactor and perform the hydrothermal reaction at 200℃ for 10h. After centrifuging the obtained reaction product, wash it with deionized water and anhydrous ethanol, and finally vacuum dry it at 60℃ to obtain the composite nano-absorbing material based on polyquinone polymers described in this invention.
[0033] The composite nano-absorbing material based on multi-quinone polymers prepared in Example 1 was characterized and its absorption performance was tested.
[0034] Figure 1 The X-ray diffraction pattern of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1 is shown. Figure 1 As shown, in addition to the typical "bulging" diffraction peaks of polymer materials appearing near 20 degrees, diffraction peaks of iron(II,III) oxide (Fe3O4, PDF#79-0419) also appear on the diffraction pattern, indicating that the sample prepared in Example 1 contains polyquinone polymers and iron(II,III) oxide.
[0035] Figure 2 This is a scanning electron microscope (SEM) image of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1. Figure 2 As shown, spherical iron oxide nanoparticles with a particle size of approximately 100 nm are uniformly distributed on the surface of the polyquinone polymer, indicating that Example 1 successfully prepared a nanocomposite material of iron oxide and polyquinone polymer with uniform composition.
[0036] Figure 3 The hysteresis loop is the magnetic field line of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1. Figure 3As shown, the measured hysteresis loop exhibits a distinct S-shaped characteristic, a typical feature of hysteresis loops in ferromagnetic materials. The saturation magnetic induction intensity (M...) s The concentration is approximately 58.1 emu / g, and the coercivity (H) is... c The result is approximately 20 Oe, indicating that the iron oxide in the sample prepared in Example 1 effectively improves the magnetic properties of the composite nano-absorbing material based on polyquinone polymers, transforming it from a non-magnetic material into a ferromagnetic polymer composite material.
[0037] The microwave absorption performance of a composite nanomaterial based on polyquinone polymers was tested using a vector network analyzer (model 3656D, manufactured by CETC Science & Technology Co., Ltd.) via the coaxial transmission line method. The test frequency range was 2.0-18.0 GHz. Before testing, the composite nanomaterial based on polyquinone polymers was mixed with paraffin wax at a mass ratio of 4:6 and pressed into a ring with an outer diameter of 7.00 mm, an inner diameter of 3.00 mm, and a thickness of approximately 3.00 mm. The ring was then placed in a fixture to test the dielectric constant (ε = ε′ - jε″) and permeability (μ = μ′ - jμ″). Based on transmission line theory, the reflection loss (RL), which reflects the microwave absorption performance, was calculated using the following formula:
[0038]
[0039] In the formula: Z in Here, f is the incident impedance, d is the electromagnetic wave frequency, c is the material thickness, and j is an imaginary number. Generally speaking, when the reflection loss is -10dB, 90% of the incident electromagnetic wave is absorbed. The frequency range where the reflection loss is less than -10dB is called the absorption bandwidth. The magnitude of the reflection loss represents the absorption intensity of the material for the incident electromagnetic wave.
[0040] Figure 4 This refers to the reflection loss of the composite nano-absorbing material based on multi-quinone polymers prepared in Example 1. For example... Figure 4 As shown, when the material thickness varies within the range of 1.0-4.5 mm, the reflection loss of this composite nano-absorbing material changes accordingly. Figure 4 As can be seen, when the thickness is 1.5 mm, the maximum absorption bandwidth of the composite nano-absorbing material based on polyquinone polymers prepared in Example 1 is 4.7 GHz (13.2-17.9 GHz), and the maximum absorption intensity is -46.6 dB. By changing the thickness, absorption performance can be achieved in a specific frequency band.
[0041] Example 2
[0042] Unlike Example 1, in step 2) of this example, 0.53g of ferric chloride was replaced with 0.42g of cobalt chloride. All other raw materials and methods were the same as in Example 1. The composite nano-absorbing material based on polyquinone polymers prepared in Example 2 had a maximum absorption bandwidth of 3.5GHz when the thickness was 1.5mm and a maximum absorption intensity of -35.7dB when the thickness was 3.3mm. Compared to Example 1, the magnetic loss capability of cobalt oxide in the composite nano-absorbing material based on polyquinone polymers prepared in Example 2 was weaker than that of iron(III) oxide, resulting in a decrease in the absorption performance of the composite nano-absorbing material.
[0043] Example 3
[0044] Unlike Example 1, in step 2) of this example, the amount of polyquinone polymer powder added is 0.3g. All other raw materials and methods are the same as in Example 1. In Example 3, the maximum absorption bandwidth is 3.2GHz when the thickness is 1.5mm, and the maximum absorption intensity is -27.4dB when the thickness is 4.0mm. Compared to Example 1, the reduced amount of polyquinone polymer powder in Example 3 results in a decrease in the relative polymer content in the final composite nano-absorbing material based on polyquinone polymers, thus reducing the absorption performance of the composite nano-absorbing material.
[0045] Example 4
[0046] Unlike Example 1, in step 2) of this example, 40 mL of ethylene glycol was replaced with 40 mL of deionized water. All other raw materials and methods were the same as in Example 1. In Example 4, the maximum absorption bandwidth was 3.3 GHz when the thickness was 1.5 mm, and the maximum absorption intensity was -26.8 dB when the thickness was 2.9 mm. Compared to Example 1, replacing ethylene glycol with deionized water in Example 4 reduced the solution viscosity, leading to irregular morphology of the product. This affected the uniform loading of iron oxide nanoparticles on the surface of the polyquinone polymer, thus reducing the absorption performance of the composite nano-absorbing material.
[0047] Examples 5-7
[0048] Unlike Example 1, the amount of ferric chloride added in Examples 5-7 was 0.27g, 0.80g and 1.06g respectively, while other reaction conditions or amounts added were the same as in Example 1.
[0049] Comparative Example 1
[0050] Unlike Example 1, the amount of ferric chloride added in Comparative Example 1 was 0g, while other reaction conditions or amounts added were the same as in Example 1.
[0051] The loading of ferric oxide directly depends on the concentration of ferric chloride solution during the hydrothermal reaction. By changing the amount of ferric chloride added in Example 1 to 0 g, 0.27 g, 0.80 g, and 1.06 g, the reflection losses of the composite nano-absorbing materials based on polyquinone polymers prepared in Examples 5-7 and Comparative Example 1 are shown in the attached figures. Figure 5 As shown in (a)-(d), the comparison shows that in Comparative Example 1, when no iron oxide is loaded, the maximum absorption bandwidth that the polyquinone polymer can achieve when the absorbing coating thickness is 2.00 mm is 3.1 GHz (11.1-14.2 GHz), and the maximum absorption intensity when the coating thickness is 4.0 mm is -25.9 dB. In Examples 5-7, the maximum absorption bandwidth and maximum absorption intensity of the composite nano-absorbing materials loaded with iron oxide were significantly improved. When the amount of iron chloride added was 0.27g, the maximum absorption bandwidth was 4.5GHz (12.4-16.9GHz) and the maximum absorption intensity was -22.5dB with a coating thickness of 1.50mm. When the amount of iron chloride added was 0.80g, the maximum absorption bandwidth was 3.9GHz (14.0-17.9GHz) with a coating thickness of 1.50mm and the maximum absorption intensity was -43.2dB with a coating thickness of 3.0mm. When the amount of iron chloride added was 1.06g, the maximum absorption bandwidth was 1.9GHz (16.0-17.9GHz) with a coating thickness of 4.50mm and the maximum absorption intensity was -16.3dB with a coating thickness of 4.0mm. In comparison, in Example 1, when the amount of ferric chloride added was 0.53g, the maximum absorption bandwidth achieved was 4.7GHz (13.2-17.9GHz) and the maximum absorption intensity was -46.6dB with a coating thickness of only 1.50mm. This means that this condition can achieve wider and stronger absorption performance with a thinner coating thickness. Too much or too little ferric chloride directly determines whether there is too much or too little iron tetroxide in the composite nano-absorbing material based on polyquinone polymers, both of which are detrimental to achieving optimal absorption performance.
[0052] Comparative Example 2
[0053] The literature RSC Adv. 2013, 3, 22554-22559 describes the preparation of polyaniline / ferric oxide composite materials using in-situ polymerization. The specific method is as follows: First, 5.56 g of ferric sulfate heptahydrate and 2 mL of hydrazine hydrate were dissolved in 100 mL of deionized water. The pH was adjusted to 9-10 using sodium hydroxide solution (1 mol / L). After thorough stirring, the mixture was placed in a reaction vessel and reacted at 180 °C for 6 h. The product was washed with deionized water and anhydrous ethanol and then dried to obtain ferric oxide powder. Next, 1 g of ferric oxide, 1 mL of dodecylbenzenesulfonic acid, and 1 mL of hydrochloric acid were added to 100 mL of deionized water. 1 mol / L ammonium persulfate and 2 mL of aniline monomer were placed in an ice-water bath at 0°C and stirred. Separately, 1.5 g of ammonium persulfate and 2 mL of hydrochloric acid solution (1 mol / L) were dissolved in 50 mL of deionized water and slowly added to the above-prepared solution. After stirring thoroughly for 10 h, the precipitate was washed with acetone and dried at 70°C for 4 h to obtain a polyaniline / ferric oxide composite material. After being compounded with paraffin at a ratio of 40 wt%, the sample was pressed to test its microwave absorption performance. When the coating thickness was 1.7 mm, a maximum absorption bandwidth of 2.7 GHz (13.6-16.3 GHz) and a maximum absorption intensity of -35.1 dB were achieved.
[0054] Comparative Example 3
[0055] The polyaniline / ferric oxide composite material prepared by the hard template method in the literature React. Funct. Polym. 2009, 69, 137–144 is as follows: First, 2.293 g of ferric sulfate heptahydrate and 5.980 g of ferric nitrate nonahydrate were dissolved in 100 mL of water, 10 mL of ammonia was quickly added, and then 1.26 g of oleic acid was added and stirred for 1 h. The ferric oxide nanoparticles were separated by magnetic adsorption, washed, and transferred to an aqueous solution of sodium dodecylbenzenesulfonate (denoted as product A). Second, 6 g of polystyrene core-shell particles sulfonated with 40 mL of concentrated sulfuric acid were used as a template, and then... 0.03 mol of aniline monomer and 0.03 mol of ammonium persulfate were added and reacted for 8 hours. After dissolving polystyrene in tetrahydrofuran, hollow polyaniline (denoted as product B) was obtained. Finally, product B and 15 mL of product A were added to 50 mL of water and reacted for 12 hours. After filtration and washing, the product was vacuum dried at 45 °C for 24 hours to obtain a polyaniline / ferric oxide composite material. The composite material was compounded with paraffin at a ratio of 75 wt% and then pressed into a sample for microwave absorption performance testing. With a coating thickness of 3.0 mm, a maximum absorption bandwidth of 2.7 GHz (7.8-10.5 GHz) and a maximum absorption intensity of -31.3 dB were achieved.
[0056] Comparative Example 4
[0057] The polypyrrole / ferric oxide composite material prepared by in-situ polymerization in the literature J. Alloys Compd. 2011, 509, 4104-4107 is as follows: First, 1 mmol of ferric chloride hexahydrate and 10 mmol of sodium acetate were dissolved in 8 mL of ethylene glycol and then transferred to a 50 mL reactor. After reacting at 180 °C for 24 h, ferric oxide powder was obtained. Then, 0.2 mmol of ferric oxide powder was ultrasonically dispersed in 40 mL of water, and 0.2 mL of pyrrole monomer was added. After sonication for 30 minutes, 10 mL of ammonium persulfate solution (1 mmol / L) was slowly added, and the mixture was stirred and reacted for 24 hours. The product was centrifuged and washed with water and anhydrous ethanol. After vacuum drying at 60 °C for 4 hours, polypyrrole / ferric oxide composite material was obtained. After being compounded with paraffin at a ratio of 50 wt%, the composite material was pressed into a sample for microwave absorption performance testing. When the coating thickness was 2.3 mm, the maximum absorption bandwidth was 5 GHz (10.5-15.5 GHz) and the maximum absorption intensity was -22.4 dB.
[0058] Compared with the material systems in Comparative Examples 2-4, the composite nano-absorbing material based on multi-quinone polymers prepared in this invention can achieve wider and stronger absorption performance with a thinner coating thickness. Furthermore, the significant difference between this invention and the preparation processes reported in Comparative Examples 2-4 is that the aforementioned documents use magnetic component iron oxide as a carrier to prepare composite materials through in-situ polymerization of organic monomers on the surface of inorganic materials; this invention uses multi-quinone polymers as a matrix, and utilizes hydrothermal reactions to achieve the nucleation and growth of iron oxide nanoparticles on the polymer surface, thereby obtaining a magnetic component-modified composite nano-absorbing material based on multi-quinone polymers.
[0059] Although the present invention has been described in detail with reference to the accompanying drawings and preferred embodiments, the invention is not limited thereto. Various equivalent modifications or substitutions can be made to the embodiments of the invention by those skilled in the art without departing from the spirit and essence of the invention, and such modifications or substitutions should all be within the scope of the invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.
Claims
1. A method for preparing a composite type nano wave-absorbing material based on a multi-province and quinone polymer, characterized in that, The preparation method comprises the following steps: 1) preparing a pyromellitenequinone polymer by a solid phase reaction method: using anthraquinone and pyromellitic dianhydride as raw materials, and a Lewis acid as a catalyst, mixing them uniformly, and then baking them in an inert atmosphere, purifying, drying, and grinding to obtain the pyromellitenequinone polymer; 2) loading nano magnetic particles on the surface of the pyromellitenequinone polymer prepared in step 1) by a hydrothermal method: dissolving a ferromagnetic metal salt in a solvent, adding polyethylene glycol 1000 monomethyl ether and sodium acetate, stirring to form a uniform solution, placing the pyromellitenequinone polymer powder obtained in step 1) in the solution, ultrasonically dispersing it uniformly, and then performing a hydrothermal reaction, centrifuging, and drying to obtain the composite nano wave-absorbing material based on the pyromellitenequinone polymer; The molar ratio of anthraquinone, pyromellitic dianhydride and the Lewis acid is 1:1:1-2; The baking in step 1) is baking at 300-330 ℃ in an inert atmosphere for 6-24 h; The purification in step 1) is extracting with 10% hydrochloric acid solution, deionized water, anhydrous ethanol and toluene respectively in a Soxhlet extractor for 12-24 h, and the drying is vacuum drying at 60-80 ℃; In step 2), 0.53-0.8 g of the ferromagnetic metal salt is dissolved in 20-100 mL of the solvent, 0.2-1.0 g of polyethylene glycol 1000 monomethyl ether and 0.6-1.5 g of sodium acetate are added, and the mixture is stirred to form a uniform solution; then 0.4 g of the pyromellitenequinone polymer powder obtained in step 1) is placed in the solution, and ultrasonic dispersion is performed for 0.5-2 h to fully disperse the pyromellitenequinone polymer powder in the solution; the solution is transferred to a hydrothermal reaction kettle, the hydrothermal reaction temperature is 200-220 ℃, and the hydrothermal reaction time is 10-24 h; the obtained reaction product is centrifuged, washed with deionized water and anhydrous ethanol, and finally vacuum dried at 60-80 ℃ to obtain the composite nano wave-absorbing material based on the pyromellitenequinone polymer; The ferromagnetic metal salt is iron chloride; The solvent is ethylene glycol.
2. The method for preparing the multi-province and quinone-based composite nano-wave-absorbing material according to claim 1, characterized in that, The Lewis acid is one of zinc chloride or aluminum chloride.
3. The method for preparing multi-province and quinone-based composite nano-wave-absorbing material according to claim 1, characterized in that, In step 1), the inert atmosphere is one of nitrogen or argon.
4. The composite nano wave-absorbing material based on the pyromellitenequinone polymer prepared by the preparation method of the composite nano wave-absorbing material based on the pyromellitenequinone polymer according to any one of claims 1-3.
Citation Information
Patent Citations
Preparation method of barium ferrite-ferroferric oxide composite wave-absorbing material
CN106587167A