CN114685975A - Wave-absorbing composite material and preparation method thereof - Google Patents
Wave-absorbing composite material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 39
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- 238000002156 mixing Methods 0.000 claims abstract description 55
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- 229920005989 resin Polymers 0.000 claims abstract description 28
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- 239000003607 modifier Substances 0.000 claims abstract description 26
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- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 29
- 239000000843 powder Substances 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 21
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
- C08J5/08—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials glass fibres
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- Polymers & Plastics (AREA)
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Abstract
The invention provides a wave-absorbing composite material and a preparation method thereof. The preparation method comprises the following steps: coating silicon dioxide on the surface of the magnetic metal particles to obtain modified magnetic metal particles; modifying the glass fiber by adopting a surface modifier comprising a silane coupling agent and ethanol to obtain modified glass fiber; and mixing the modified magnetic metal particles, the modified glass fiber and the resin master batch to obtain the wave-absorbing composite material. Through modification of the magnetic metal particles, the silicon dioxide is coated on the surfaces of the magnetic metal particles, so that the polarity of the surfaces of the magnetic metal particles is reduced, the dispersity of the magnetic metal particles in nylon is improved, and the shock resistance of the material is improved while the wave absorption performance is improved; and the glass fiber is subjected to surface treatment and then is dispersed in the resin in a blending mode, so that the glass fiber and the wave absorbing agent play a role in synergistic toughening, and the tensile strength of the material is improved by adding the glass fiber.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a wave-absorbing composite material and a preparation method thereof.
Background
With the rapid development of modern social economy, the change of electronic information technology and the continuous progress of science and technology, people have qualitative leap in clothes, eating, living and going, and many people have bet their eyes on higher-quality life while exclamating the beauty of the current life. However, the current social problems of environmental pollution, food safety, electromagnetic radiation and the like are attracting more and more attention. In particular, electromagnetic devices are increasingly used, and are small in size, such as mobile communication, computers, household appliances, large in size, production equipment, aerospace and the like. In recent years, reports on the harm of electromagnetic radiation to human health are frequent. Researches show that electromagnetic radiation has harm to organisms, most people live in the electromagnetic radiation from cables and household appliances for a long time, the risk coefficient of human suffering from cancers and degenerative diseases is continuously increased, particularly, the electromagnetic wave with higher frequency has higher harm to human bodies, has obvious harm to the cells of organisms, nervous systems, reproduction and metabolism functions of new materials, and has stronger penetrating power and even can strongly interfere military equipment, precise medical instruments, aerospace facilities and the like. Therefore, the research and preparation of the composite material with the wave absorption performance has very important significance in the aspects of absorbing, protecting, weakening the harm of electromagnetic radiation to human health, protecting the life of people and the like.
Disclosure of Invention
The invention mainly aims to provide a wave-absorbing composite material and a preparation method thereof, and aims to solve the problem that electromagnetic radiation harms human health in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a wave-absorbing composite material, comprising the steps of: coating silicon dioxide on the surface of the magnetic metal particles to obtain modified magnetic metal particles; modifying the glass fiber by adopting a surface modifier comprising a silane coupling agent and ethanol to obtain modified glass fiber; and mixing the modified magnetic metal particles, the modified glass fiber and the resin master batch to obtain the wave-absorbing composite material.
Further, the step of coating the magnetic metal particles with silica comprises: dispersing magnetic metal particles in ethanol to obtain a dispersion liquid; mixing methyl orthosilicate, ammonia water and water with the dispersion liquid, reacting to hydrolyze and condense the methyl orthosilicate to form silicon dioxide wrapping the magnetic metal particles, and thus obtaining the modified magnetic metal particles, wherein the volume ratio of the methyl orthosilicate to the ammonia water to the water is (0.5-1): (0.1-0.5): (2-4), preferably, the temperature for hydrolyzing and condensing the methyl orthosilicate is 80-85 ℃, and the time is 5-8 h.
Further, before the step of coating the magnetic metal particle with the silica, the preparation method further comprises the steps of: the magnetic metal particles are pulverized into a flake form, and preferably the width of any horizontal cross section of the flake-form magnetic metal particles is 60 to 300 nm.
Further, the magnetic metal particles are hydroxyl iron powder.
Further, before the step of coating the surface of the magnetic metal particles with silicon dioxide, the preparation method further comprises the step of pretreating the magnetic metal particles as follows: mixing a bluing agent and the solution dispersed with the magnetic metal particles, and reacting to obtain a mixed solution, wherein the reaction temperature is preferably 80-85 ℃, and the reaction time is 2-4 hours; and (4) carrying out solid-liquid separation on the mixed solution, wherein the solid phase is the pretreated magnetic metal particles.
Further, the step of modifying the glass fibers comprises: preparing a silane coupling agent, water and ethanol into a surface modifier, preferably selecting the silane coupling agent, the water and the ethanol in a weight ratio of (1-2): (0.1-0.5): (0.5 to 1); diluting a surface modifier, wherein the preferred diluent is acetone; impregnating the glass fiber with the diluted surface modifier, and drying the glass fiber.
Further, in the step of mixing, the weight ratio of the modified magnetic metal particles, the modified glass fibers and the resin master batch is (3-12): (9-24): 1, preferably mixing for 5-15 min, preferably after the mixing step, and the preparation method further comprises the step of sequentially standing and back-mixing the mixed product, preferably standing for 1-5 min and back-mixing for 5-15 min.
Further, in the step of mixing, the modified magnetic metal particles, the modified glass fibers and the resin master batch are added into a torque rheometer for mixing, and preferably, the torque of the torque rheometer is 30-80 r/min.
Further, the resin masterbatch is polyhexamethylene adipamide.
According to another aspect of the invention, the wave-absorbing composite material is prepared by the preparation method.
The technical scheme of the invention is applied to provide the wave-absorbing composite material and the preparation method thereof, the glass fiber reinforced wave-absorbing composite material is prepared by a blending method, wherein the glass fiber is modified to increase the compatibility with resin, so that the tensile strength of the material is increased; meanwhile, the silicon dioxide is coated on the surface of the magnetic metal particles, so that the dispersion of the wave-absorbing material in the matrix is improved, the wave-absorbing performance and the impact resistance of the composite material are improved, the composite material with the wave-absorbing performance is researched, and the harm of electromagnetic radiation to human health can be absorbed, protected and weakened.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and in the claims of the present invention are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As introduced in the background art, research and preparation of the composite material with the wave absorption performance has very important significance in the aspects of absorbing, protecting, weakening the harm of electromagnetic radiation to human health, protecting human life and the like.
In order to solve the technical problems, the application provides a preparation method of a wave-absorbing composite material, which comprises the following steps: coating silicon dioxide on the surface of the magnetic metal particles to obtain modified magnetic metal particles; modifying the glass fiber by adopting a surface modifier comprising a silane coupling agent and ethanol to obtain modified glass fiber; and mixing the modified magnetic metal particles, the modified glass fiber and the resin master batch to obtain the wave-absorbing composite material.
The conventional nylon resin does not have wave-absorbing performance, in order to achieve the purpose, the composite material has certain wave-absorbing performance by adding the wave-absorbing agent into the nylon resin, and the dispersion degree of the wave-absorbing agent in a nylon resin matrix is increased by carrying out surface treatment on the wave-absorbing agent, so that the wave-absorbing performance and the mechanical property of the composite material are further improved.
The prepared wave-absorbing composite material has poor impact property and low tensile strength, and in order to further improve the mechanical property of the material, the mechanical property of the material is improved by adding the glass fiber, but the polarity of the glass fiber is stronger, and in order to reduce the surface energy of the glass fiber, the surface treatment is carried out, so that the glass fiber and the wave-absorbing agent generate synergy, and the mechanical property of the material is further improved.
The preparation method of the invention prepares the glass fiber reinforced wave-absorbing composite material by a blending method, wherein the compatibility of the glass fiber reinforced wave-absorbing composite material with resin is increased by modifying the glass fiber, so that the tensile strength of the material is increased; meanwhile, the silicon dioxide is coated on the surface of the magnetic metal particles, so that the dispersion of the wave-absorbing material in the matrix is improved, the wave-absorbing performance and the impact resistance of the composite material are improved, the composite material with the wave-absorbing performance is researched, and the harm of electromagnetic radiation to human health can be absorbed, protected and weakened.
An exemplary embodiment of a method of making a wave-absorbing composite material provided in accordance with the present invention will now be described in more detail. These exemplary embodiments may, however, be embodied in many different forms and should not be construed as limited to only the embodiments set forth herein. It should be understood that these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the concept of these exemplary embodiments to those skilled in the art.
Firstly, coating silicon dioxide on the surface of magnetic metal particles to obtain modified magnetic metal particles, and modifying glass fibers by adopting a surface modifier comprising a silane coupling agent and ethanol to obtain modified glass fibers. The magnetic metal particles may be iron powder.
In a preferred embodiment, the step of coating the magnetic metal particles with silica comprises: dispersing magnetic metal particles in ethanol to obtain a dispersion liquid; mixing methyl orthosilicate, ammonia water and water with the dispersion liquid and reacting to hydrolyze and condense the methyl orthosilicate to form silicon dioxide wrapping the magnetic metal particles, thereby obtaining the modified magnetic metal particles.
In the above preferred embodiment, the method of forming the silica coating is a conventional Stober method, which is a commonly used method for preparing a monodisperse silica shell, and the principle thereof is That Methyl Orthosilicate (TMOS) is catalyzed by ammonia water in an alcohol phase medium, and hydrolysis-condensation is performed to generate monodisperse silica ions, which has advantages of simple process conditions, less side reactions, and high purity of the prepared product.
In order to improve the coating effect of the silicon dioxide on the magnetic metal particles, the volume ratio of The Methyl Orthosilicate (TMOS), the ammonia water and the water is more preferably (0.5-1): (0.1-0.5): (2-4).
In order to improve the efficiency of hydrolyzing and condensing the methyl orthosilicate, the reaction time of the methyl orthosilicate, the ammonia water and the water with the dispersion liquid is more preferably 80-85 ℃ and is 5-8 hours.
In order to improve the coating effect of the silicon dioxide on the magnetic metal particles, before the step of coating the silicon dioxide on the surfaces of the magnetic metal particles, the preparation method of the invention may further comprise the following steps: the magnetic metal particles are pulverized into a flake form, and preferably, the width of any horizontal cross section of the flake-form magnetic metal particles is 60 to 300 nm.
In a preferred embodiment, the above preparation method of the present invention further comprises, before the step of coating the surface of the magnetic metal particles with silica, the step of subjecting the magnetic metal particles to the following pretreatment: mixing and reacting a bluing agent with a solution dispersed with magnetic metal particles to obtain a mixed solution; and (4) carrying out solid-liquid separation on the mixed solution, wherein the solid phase is the pretreated magnetic metal particles.
In order to improve the reaction efficiency of the bluing agent and the solution dispersed with the magnetic metal particles, the reaction is preferably carried out at 80-85 ℃ for 2-4 hours.
In the preferred embodiment, the pH of the solution is adjusted to about 9 by adding an appropriate amount of ammonia water to provide a slightly alkaline environment to facilitate the reaction, the reaction temperature, and the amount of the bluing agent is controlled to prepare the iron powder with a core-shell structure, so that the iron powder is more easily dispersed in the resin matrix.
In a preferred embodiment, the step of modifying the glass fibers comprises: preparing a silane coupling agent, water and ethanol into a surface modifier; diluting the surface modifier; impregnating the glass fiber with the diluted surface modifier, and drying the glass fiber.
In order to further increase hydroxyl groups on the surface of the glass fiber and thus enhance the tensile strength and impact resistance of the composite material by reducing the polarity of the glass fiber, the weight ratio of the silane coupling agent to water to ethanol is more preferably (1-2): (0.1-0.5): (0.5-1), the diluent can be acetone; more preferably, the glass fiber is impregnated for 10 to 15 hours.
And after the steps of preparing and obtaining the modified magnetic metal particles and the modified glass fibers, mixing the modified magnetic metal particles, the modified glass fibers and the resin master batch to obtain the wave-absorbing composite material.
The glass fiber has high strength and high Young's modulus, each fiber bundle consists of hundreds or even thousands of monofilaments, the glass fiber is non-combustible, heat-resistant and corrosion-resistant, and has low water absorption rate, so that the glass fiber can be used as a composite material reinforcement. In addition, the glass fiber is modified, so that the compatibility of the glass fiber and resin is improved, and the tensile strength of the composite material is further improved.
Specifically, the glass fiber is dispersed in the resin matrix, the root part of the glass fiber is tightly combined with the resin, the glass fiber exposed on the surface of the glass fiber has a large amount of resin matrix, when the glass fiber receives external impact, the glass fiber can well disperse impact and is not easy to be debonded from the matrix, so that the acting force is concentrated on the material, the crack generated when the material is damaged is diffused to the boundary, and the brittle fracture is presented, thereby improving the impact resistance of the material.
Meanwhile, the silicon dioxide is coated on the surface of the magnetic metal particles, so that the dispersion of the wave-absorbing material in the matrix is improved, and the wave-absorbing performance and the shock resistance of the composite material are improved.
Preferably, the resin masterbatch is polyhexamethylene adipamide (nylon 66). Nylon 66 is a widely used plastic which is prepared by polycondensation of adipic acid and hexamethylenediamine in equal proportions, and has excellent tensile and flexural properties due to orientation of the molecule under the action of hydrogen bonds, owing to the polar amide bond-containing functional group, and also has the highest yield in all nylon products. In addition, due to the characteristics of good wear resistance, easy processing and the like, the wear-resistant rubber belt has wide application in the fields of automobiles, electronics, mechanical and chemical engineering, daily products and the like.
Because nylon 66 has the defects of high water absorption, low impact property, no wave-absorbing property and the like, the use of the nylon 66 in national life is limited, and in order to enrich the application field, enhance the mechanical property and increase the wave-absorbing property of the material, the modified magnetic metal particles and the modified glass fiber are mixed with the nylon 66, so that the nylon 66 is endowed with the wave-absorbing property, and the nylon 66 also has excellent mechanical properties such as elastic modulus, impact strength, tensile strength and the like.
In order to further improve the wave absorbing performance and the mechanical property of the composite material, in the step of mixing, the weight ratio of the modified magnetic metal particles, the modified glass fibers and the resin master batch is preferably (3-12): (9-24): 1; preferably, the mixing time is 5-15 min.
In a preferred embodiment, after the step of mixing, the preparation method of the present invention further comprises the step of sequentially standing and back-mixing the mixed product, and more preferably, the standing time is 1 to 5min, and the back-mixing time is 5 to 15 min.
In order to improve the mixing efficiency, in the mixing step, the modified magnetic metal particles, the modified glass fibers and the resin master batch can be added into a torque rheometer for mixing, and the torque of the torque rheometer is preferably 30 to 80 r/min.
According to another aspect of the invention, the wave-absorbing composite material is prepared by the preparation method.
The composite material is a glass fiber reinforced wave-absorbing composite material formed by blending modified magnetic metal particles, modified glass fibers and resin master batches, wherein the glass fibers are modified to increase the compatibility of the glass fibers and resin, so that the tensile strength of the material is increased; meanwhile, the silicon dioxide is coated on the surface of the magnetic metal particles, so that the dispersion of the wave-absorbing material in the matrix is improved, the wave-absorbing performance and the impact resistance of the composite material are improved, the composite material with the wave-absorbing performance is researched, and the harm of electromagnetic radiation to human health can be absorbed, protected and weakened.
The wave-absorbing composite material and the preparation method thereof of the present invention will be further described with reference to the following examples.
Example 1
The embodiment provides a preparation method of a wave-absorbing composite material, which comprises the following steps:
1. surface treatment of iron powder with hydroxyl groups
1) And (2) carrying out ball milling on the hydroxyl iron powder by using a planetary ball mill, and grinding for 4 hours at 80 ℃ to ensure that the particle size (namely the width of any horizontal section of the sheet) of the hydroxyl iron powder meets 60-300 nm.
2) 100ml of deionized water was weighed into a 200ml beaker, and then 20ml of an alkaline bluing agent (XS 06-1, analytical pure, chemical technology Co., Ltd.) was weighed and contained in the beaker and stirred for 20 min.
3) The iron powder was placed in a three-necked flask in which 100ml of deionized water was weighed in advance, and sonicated at 30 ℃ for 30 min.
4) And after stirring is finished, placing the mixed solution containing the bluing agent into a three-neck flask which is well subjected to ultrasonic treatment, then placing the three-neck flask into a constant-temperature oil bath kettle at the temperature of 80 ℃, and stirring for 2 hours at constant temperature.
5) And pouring out the supernatant, repeatedly washing the reacted mixture precipitate for more than 5 times by using absolute ethyl alcohol, washing away unreacted bluing agent, centrifuging for 30min by using a centrifuge, drying for 6 hours in a constant-temperature oven at 80 ℃, and finally grinding and sieving the dried hydroxyl iron powder.
6) 150ml of TMOS (methyl orthosilicate) is weighed into a flask, a proper amount of sieved ferroxyl powder is weighed, and the ferroxyl powder is placed into a beaker to perform ultrasonic treatment for 30min at room temperature.
7) 300ml of deionized water and 15ml of ammonia water are uniformly mixed, then the mixture is transferred into a flask containing iron powder, and the mixture is stirred and reacts for 5 hours in a water bath kettle at constant temperature of 80 ℃. After the reaction is finished, repeatedly washing the modified hydroxyl iron powder by using absolute ethyl alcohol, removing unreacted TMOS, and then drying and grinding for later use.
2. Modification treatment of glass fibers
1) Silane coupling agent (KH-570, guangzhou polymer industries), deionized water and absolute ethyl alcohol were mixed according to the ratio of 1: 0.3: 0.7 is prepared into a surface modifier, and then a proper amount of acetone is weighed and diluted to prepare a solution with the modifier content of 1 percent.
2) Glass fiber (ECS 407-3-K, Chongqing International composite Co., Ltd.) was added to the prepared diluent and soaked for 12h.
3) And (3) drying the infiltrated glass fiber in a natural state, and then putting the glass fiber in an oven to dry 6, and taking out.
3. And (3) compounding the glass fiber reinforced wave-absorbing nylon 66 composite material.
1) And (3) placing nylon 66 (Shanghai plastic products, eighteen factories, M20), modified glass fiber and the surface-treated hydroxyl iron powder in a blast oven, and drying for 14 hours at 80 ℃.
2) Preparing nylon 66 master batch, glass fiber and surface-treated hydroxyl iron powder according to the mass ratio of 2.5: 7: 0.3, weighing the material mixing disc, uniformly stirring, setting a first area of a torque rheometer to be 250 ℃, a second area to be 255 ℃, a third area to be 260 ℃ and a fourth area to be 265 ℃, waiting for the completion of temperature rise, and adjusting the torque to be 50 r/min.
3) And adding the stirred materials into a torque rheometer for mixing, standing for 3min after mixing for about 10min, and then back mixing for 10 min. And taking out the mixed material, cooling to room temperature, drying and crushing to obtain the composite material.
Example 2
The embodiment provides a preparation method of a wave-absorbing composite material, which comprises the following steps:
1. surface treatment of iron powder with hydroxyl groups
1) And (3) carrying out ball milling on the hydroxyl iron powder by using a planetary ball mill, and grinding for 4 hours at 80 ℃ to enable the particle size of the hydroxyl iron powder to meet 60-300 nm.
2) 100ml of deionized water was weighed into a 200ml beaker, and then 20ml of bluing agent was weighed and placed in the beaker and stirred for 20 min.
3) Putting a proper amount of ferrous hydroxy powder into a three-neck flask in which 100ml of deionized water is weighed in advance, and carrying out ultrasonic treatment at 30 ℃ for 30 min.
4) And after stirring is finished, placing the mixed solution containing the bluing agent into a three-neck flask which is well subjected to ultrasonic treatment, then placing the three-neck flask into a constant-temperature oil bath kettle at the temperature of 80 ℃, and stirring for 2 hours at constant temperature.
5) And pouring out supernatant, repeatedly washing the reacted mixture precipitate for more than 5 times by using absolute ethyl alcohol, washing away unreacted bluing agent, centrifuging for 30min by using a centrifuge, drying for 6 hours in a constant-temperature oven at the temperature of 80 ℃, and finally grinding and sieving the dried hydroxyl iron powder.
6) 150ml of TMOS (methyl orthosilicate) is weighed into a flask, a proper amount of sieved ferroxyl powder is weighed, and the ferroxyl powder is placed into a beaker to perform ultrasonic treatment for 30min at room temperature.
7) 300ml of deionized water and 15ml of ammonia water are uniformly mixed, then the mixture is transferred into a flask containing iron powder, and the mixture is stirred and reacts for 5 hours in a water bath kettle at constant temperature of 80 ℃. After the reaction is finished, repeatedly washing the modified hydroxyl iron powder by using absolute ethyl alcohol, removing unreacted TMOS, and then drying and grinding for later use.
2. Modification treatment of glass fibers
1) Silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 1: 0.3: 0.7 is prepared into a surface modifier, and then a proper amount of acetone is weighed and diluted to prepare a solution with the modifier content of 1 percent.
2) Adding the glass fiber into the prepared diluent, and soaking for 12h.
3) And (3) airing the soaked glass fibers in a natural state, and then putting the glass fibers in an oven for drying 6 and taking out.
3. And (3) compounding the glass fiber reinforced wave-absorbing nylon 66 composite material.
1) And (3) placing the nylon 66, the modified glass fiber and the surface-treated hydroxyl iron powder in a blast oven, and drying for 14 hours at the temperature of 80 ℃.
2) Preparing nylon 66 master batch, glass fiber and surface-treated hydroxyl iron powder according to the mass ratio of 3: 7: 0.5, weighing the material mixing disc, uniformly stirring, setting the first area of the torque rheometer to be 250 ℃, 255 ℃, the third area to be 260 ℃ and the fourth area to be 265 ℃, waiting for the completion of temperature rise, and adjusting the torque to be 50 r/min.
3) And adding the stirred materials into a torque rheometer for mixing, standing for 3min after mixing for about 10min, and then back mixing for 10 min. And taking out the mixed material, cooling to room temperature, drying and crushing to obtain the composite material.
Example 3
The embodiment provides a preparation method of a wave-absorbing composite material, which comprises the following steps:
1. surface treatment of iron powder with hydroxyl groups
1) And (3) carrying out ball milling on the hydroxyl iron powder by using a planetary ball mill, and grinding for 4 hours at 80 ℃ to enable the particle size of the hydroxyl iron powder to meet 60-300 nm.
2) 100ml of deionized water was weighed into a 200ml beaker, and then 20ml of bluing agent was weighed and placed in the beaker and stirred for 20 min.
3) Putting a proper amount of ferrous hydroxy powder into a three-neck flask in which 100ml of deionized water is weighed in advance, and carrying out ultrasonic treatment at 30 ℃ for 30 min.
4) And after stirring is finished, placing the mixed solution containing the bluing agent into a three-neck flask which is well subjected to ultrasonic treatment, then placing the three-neck flask into a constant-temperature oil bath kettle at the temperature of 80 ℃, and stirring for 2 hours at constant temperature.
5) And pouring out the supernatant, repeatedly washing the reacted mixture precipitate for more than 5 times by using absolute ethyl alcohol, washing away unreacted bluing agent, centrifuging for 30min by using a centrifuge, drying for 6 hours in a constant-temperature oven at 80 ℃, and finally grinding and sieving the dried hydroxyl iron powder.
6) 150ml of TMOS (methyl orthosilicate) is weighed into a flask, a proper amount of sieved ferroxyl powder is weighed, and the ferroxyl powder is placed into a beaker to perform ultrasonic treatment for 30min at room temperature.
7) 300ml of deionized water and 15ml of ammonia water are uniformly mixed, then the mixture is transferred into a flask containing iron powder, and the mixture is stirred and reacts for 5 hours in a water bath kettle at constant temperature of 80 ℃. After the reaction is finished, repeatedly washing the modified hydroxyl iron powder by using absolute ethyl alcohol, removing unreacted TMOS, and then drying and grinding for later use.
2. Modification treatment of glass fibers
1) Silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 1: 0.3: 0.7 is prepared into a surface modifier, and then a proper amount of acetone is weighed and diluted to prepare a solution with the modifier content of 1 percent.
2) Adding the glass fiber into the prepared diluent, and soaking for 12h.
3) And (3) airing the soaked glass fibers in a natural state, and then putting the glass fibers in an oven for drying 6 and taking out.
3. And (3) compounding the glass fiber reinforced wave-absorbing nylon 66 composite material.
1) And (3) placing the nylon 66, the modified glass fiber and the surface-treated hydroxyl iron powder in a blast oven, and drying for 14 hours at the temperature of 80 ℃.
2) Preparing nylon 66 master batch, glass fiber and surface-treated hydroxyl iron powder according to the mass ratio of 3.5: 6.5: 0.7, weighing the material mixing disc, uniformly stirring, setting the first area of the torque rheometer to be 250 ℃, 255 ℃, the third area to be 260 ℃ and the fourth area to be 265 ℃, waiting for the completion of temperature rise, and adjusting the torque to be 50 r/min.
3) And adding the stirred materials into a torque rheometer for mixing, standing for 3min after mixing for about 10min, and then back mixing for 10 min. And taking out the mixed material, cooling to room temperature, drying and crushing to obtain the composite material.
Example 4
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
weighing 15ml of TMOS (methyl orthosilicate) in a flask;
120ml of deionized water and 15ml of ammonia water were mixed uniformly and transferred to a flask containing iron powder.
Example 5
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
225ml of TMOS (methyl orthosilicate) was weighed into a flask;
300ml of deionized water and 15ml of ammonia water were mixed well and transferred to a flask containing iron powder.
Example 6
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
the deionized water and ammonia water are mixed evenly, then transferred into a flask containing iron powder, and stirred and reacted for 8 hours in a water bath kettle at constant temperature of 85 ℃.
Example 7
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
and after stirring is finished, placing the mixed solution containing the bluing agent into a three-neck flask which is well subjected to ultrasonic treatment, then placing the three-neck flask into a constant-temperature oil bath kettle at 85 ℃, and stirring for 4 hours at constant temperature.
Example 8
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 1: 0.1: 0.5 is configured as a surface modifier.
Example 9
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 2: 0.5: 1 is configured as a surface modifier.
Example 10
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 2: 0.5: 1 is configured as a surface modifier.
Example 11
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 3: 9: 1 is configured as a surface modifier.
Example 12
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the proportion of 12: 24: 1 is configured as a surface modifier.
Example 13
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
silane coupling agent, deionized water and absolute ethyl alcohol are mixed according to the weight ratio of 15: 9: 1 is configured as a surface modifier.
Example 14
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
and adding the stirred materials into a torque rheometer for mixing, standing for 1min after mixing for about 5min, and then back mixing for 5 min. And taking out the mixed material, cooling to room temperature, drying and crushing to obtain the composite material.
Example 15
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
and adding the stirred materials into a torque rheometer for mixing, mixing for about 15min, standing for 5min, and then back-mixing for 15 min. And taking out the mixed material, cooling to room temperature, drying and crushing to obtain the composite material.
Example 16
The difference between the preparation method of the wave composite material provided in this example and example 1 is that:
and adding the stirred materials into a torque rheometer for mixing, taking out the mixed materials after mixing for about 10min, cooling to room temperature, drying and crushing to obtain the composite material.
And pressing the mixed nylon 66 composite material into a standard tensile sample and an impact sample by using a vacuum film pressing machine. Then, the tensile properties of the materials were measured using an electronic universal tester, and the impact resistance of the materials was measured using an impact tester, and the test results are shown in table 1.
TABLE 1
The composite material is made into an annular sample with the outer diameter of 7.00mm, the inner diameter of 3.04mm and the thickness of about 2mm, the complex dielectric constant and the complex permeability of the annular sample in the frequency range of 2-18 GHz are tested on a vector network analyzer, the microwave absorption performance of the material is calculated and analyzed according to a transmission line simulation theory, and the test result is shown in table 2.
TABLE 2
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
the glass fiber reinforced wave-absorbing composite material is prepared by a blending method, wherein the compatibility of the glass fiber reinforced wave-absorbing composite material with resin is improved by modifying the glass fiber, so that the wave-absorbing performance and the tensile property of the composite material are enhanced by improving the dispersibility of the glass fiber reinforced wave-absorbing composite material in a matrix; meanwhile, the silicon dioxide is coated on the surface of the magnetic metal particles, so that the dispersion of the wave-absorbing material in the matrix is improved, the wave-absorbing performance and the impact resistance of the composite material are improved, the composite material with the wave-absorbing performance is researched, and the harm of electromagnetic radiation to human health can be absorbed, protected and weakened.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the wave-absorbing composite material is characterized by comprising the following steps of:
coating silicon dioxide on the surface of the magnetic metal particles to obtain modified magnetic metal particles;
modifying the glass fiber by adopting a surface modifier comprising a silane coupling agent and ethanol to obtain modified glass fiber;
and mixing the modified magnetic metal particles, the modified glass fibers and the resin master batch to obtain the wave-absorbing composite material.
2. The method according to claim 1, wherein the step of coating the magnetic metal particles with the silica comprises:
dispersing the magnetic metal particles in ethanol to obtain a dispersion liquid;
mixing methyl orthosilicate, ammonia water and water with the dispersion liquid, and reacting to hydrolyze and condense the methyl orthosilicate to form silicon dioxide wrapping the magnetic metal particles, so as to obtain the modified magnetic metal particles, wherein the volume ratio of the methyl orthosilicate to the ammonia water to the water is preferably (0.5-1): (0.1-0.5): (2-4), preferably, the temperature of the hydrolysis condensation of the methyl orthosilicate is 80-85 ℃, and the time is 5-8 h.
3. The production method according to claim 1 or 2, characterized in that, before the step of coating the silica on the surface of the magnetic metal particles, the production method further comprises the steps of:
the magnetic metal particles are pulverized into a flake shape, and preferably the width of any horizontal cross section of the magnetic metal particles in the flake shape is 60 to 300 nm.
4. The production method according to claim 1 or 2, wherein the magnetic metal particles are iron hydroxy powder.
5. The production method according to claim 1 or 2, characterized in that, prior to the step of coating the surface of the magnetic metal particles with the silica, the production method further comprises the step of subjecting the magnetic metal particles to the following pretreatment:
mixing a bluing agent and the solution dispersed with the magnetic metal particles, and reacting to obtain a mixed solution, wherein the reaction temperature is preferably 80-85 ℃, and the reaction time is 2-4 hours;
and carrying out solid-liquid separation on the mixed solution, wherein the solid phase is the pretreated magnetic metal particles.
6. The method of claim 1 or 2, wherein the step of modifying the glass fibers comprises:
preparing the silane coupling agent, water and the ethanol into the surface modifier, wherein the weight ratio of the silane coupling agent to the water to the ethanol is (1-2): (0.1-0.5): (0.5 to 1);
diluting the surface modifier, wherein the preferred diluent is acetone;
impregnating the glass fiber with the diluted surface modifier, and drying the glass fiber.
7. The production method according to claim 1 or 2, wherein in the step of kneading, a weight ratio of the modified magnetic metal particles, the modified glass fibers, and the resin masterbatch is (3 to 12): (9-24): 1, preferably, the mixing time is 5-15 min, preferably, after the mixing step, the preparation method further comprises the step of sequentially standing and back-mixing the mixed product, preferably, the standing time is 1-5 min, and the back-mixing time is 5-15 min.
8. The production method according to claim 7, wherein in the step of kneading, the modified magnetic metal particles, the modified glass fibers and the resin masterbatch are added to a torque rheometer to be kneaded, preferably, the torque of the torque rheometer is 30 to 80 r/min.
9. The production method according to claim 1 or 2, characterized in that the resin masterbatch is polyhexamethylene adipamide.
10. A wave-absorbing composite material, characterized in that it is prepared by the preparation method of any one of claims 1 to 9.
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