CN113754911A - Environment-friendly electromagnetic shielding building material and preparation method thereof - Google Patents
Environment-friendly electromagnetic shielding building material and preparation method thereof Download PDFInfo
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- CN113754911A CN113754911A CN202111147870.8A CN202111147870A CN113754911A CN 113754911 A CN113754911 A CN 113754911A CN 202111147870 A CN202111147870 A CN 202111147870A CN 113754911 A CN113754911 A CN 113754911A
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- 239000004566 building material Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052802 copper Inorganic materials 0.000 claims abstract description 35
- 239000010949 copper Substances 0.000 claims abstract description 35
- 239000002105 nanoparticle Substances 0.000 claims abstract description 23
- 239000002033 PVDF binder Substances 0.000 claims abstract description 21
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000007613 environmental effect Effects 0.000 claims abstract description 6
- 238000007493 shaping process Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract 7
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 9
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 9
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical group CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 8
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 239000012528 membrane Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- 238000000635 electron micrograph Methods 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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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
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Complex oxides containing cobalt and at least one other metal element
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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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
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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Abstract
本发明提出了一种环保电磁屏蔽建筑材料及其制备方法，属于建筑材料技术领域。包括以下步骤：制备钴酸铜纳米颗粒；制备钴酸铜纳米颗粒与聚偏二氟乙烯复合膜；复合膜的塑形。通过水热法制备了钴酸铜纳米颗粒，利用这种钴酸铜颗粒的纳米效应和电磁特性，实现了优秀的电磁波屏蔽性能；并通过与聚偏二氟乙烯复合，形成复合的膜材料。此种复合膜在极低的复合比和厚度下可以实现较好的吸波性能，同时该种膜结构可以直接粘贴于现有房间内壁实现微波暗室，使用简单；同时制备过程中不使用除酒精外的溶剂，不产生有毒尾气，且副产物均为易处理的金属离子，具有良好的环保特性。
The invention provides an environment-friendly electromagnetic shielding building material and a preparation method thereof, belonging to the technical field of building materials. The method comprises the following steps: preparing copper cobaltate nanoparticles; preparing a composite film of copper cobaltate nanoparticles and polyvinylidene fluoride; and shaping the composite film. The copper cobaltate nanoparticles were prepared by hydrothermal method, and the excellent electromagnetic wave shielding performance was realized by utilizing the nano-effect and electromagnetic properties of the copper cobaltate particles; and the composite membrane material was formed by compounding with polyvinylidene fluoride. This kind of composite film can achieve good wave absorption performance under extremely low composite ratio and thickness, and at the same time, the film structure can be directly pasted on the inner wall of the existing room to realize a microwave darkroom, which is easy to use; at the same time, no alcohol removal is used in the preparation process. It does not produce toxic exhaust gas, and the by-products are easy-to-handle metal ions, which have good environmental protection characteristics.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an environment-friendly electromagnetic shielding building material and a preparation method of the environment-friendly electromagnetic shielding building material.
Background
The electromagnetic shielding material is a material capable of absorbing and shielding electromagnetic waves in a certain frequency band. With the continuous development of electromagnetic wave technology, the convenience of human life is remarkably improved, but the problems of confidentiality, human body protection and the like are brought. This has led to a significant increase in the need for shielding electromagnetic waves in certain environments. In the field of buildings, the demand for microwave darkrooms is greatly increased, and the demand includes not only narrowly defined microwave darkrooms applied to scientific research, but also broad confidential meeting rooms, examination rooms or other special scenes needing to isolate external electromagnetic signals. Therefore, the research on the building material with good electromagnetic shielding performance is of great significance.
In recent years, although a large amount of electromagnetic shielding building materials are put into production and use, the existing electromagnetic shielding building materials often have the problems of poor performance, large thickness, large specific gravity, difficult use, large occupied space, environmental-friendly preparation process and the like, which affect practical use.
Therefore, in order to meet the above-mentioned shortcomings and requirements of practical applications, an object of the present invention is to provide an electromagnetic shielding building material and a preparation method thereof, wherein the electromagnetic shielding building material has excellent wave-absorbing strength, a wider operating frequency band, low density, a low composite ratio, convenient use, and an environmentally friendly preparation process.
Disclosure of Invention
Aiming at the problems pointed out in the background art, the invention provides an electromagnetic shielding building material which has excellent wave-absorbing strength, wider working frequency band, low density, low composite ratio, convenient use and environment-friendly preparation process and a preparation method thereof.
The technical scheme of the invention is realized as follows:
a preparation method of an environment-friendly electromagnetic shielding building material comprises the following steps:
s1, preparing copper cobaltate nanoparticles: weighing a certain amount of cobalt nitrate and copper nitrate, mixing the cobalt nitrate and the copper nitrate with a certain amount of aqueous solution of ethanol, stirring to dissolve, adding ammonia water and hexadecyl trimethyl ammonium bromide, and stirring at room temperature; transferring the mixture to a reaction kettle, heating, centrifuging, drying, and burning in air in a crucible; carrying out secondary firing on the fired product in an argon atmosphere to obtain copper cobaltate nanoparticles;
s2, preparing a copper cobaltate nanoparticle and polyvinylidene fluoride composite membrane: mixing and heating the copper cobaltate nanoparticles prepared in the step S1 and polyvinylidene fluoride in a solvent, performing ultrasonic treatment, cooling after the mixture is uniform, and drying to obtain a copper cobaltate nanoparticle and polyvinylidene fluoride composite film;
s3, shaping of a composite film: and (4) heating the copper cobaltate nanoparticles prepared in the step (S2) and the polyvinylidene fluoride composite film in a mould, applying a certain pressure, and cooling to obtain a final composite film product.
According to an embodiment of the present invention, in the above step S1, the mixing ratio of the cobalt nitrate, the copper nitrate, the ethanol aqueous solution, the ammonia water, and the cetyltrimethylammonium bromide is: 0.291g, 0.236g, 85ml, 5ml, 0.08 g.
According to an embodiment of the present invention, in the above step S1, the ethanol aqueous solution has a concentration of 70% and the ammonia aqueous solution has a concentration of 30%.
According to an embodiment of the present invention, in the above step S1, the stirring time at room temperature is 4-6 h.
According to an embodiment of the present invention, in the step S1, the heating temperature of the reaction kettle is 90 ℃ and the heating time is 400-.
According to an embodiment of the present invention, in the above step S1, the burning temperature in the crucible is 150 ℃, the burning time is 5min, and the temperature of the secondary burning in the argon atmosphere is 400 ℃, and the time is 400 min.
According to an embodiment of the present invention, in the above step S2, the ratio of the nano copper cobaltate to the polyvinylidene fluoride is 0.01-0.05.
According to an embodiment of the present invention, in the above step S2, the solvent is acetamide.
According to an embodiment of the present invention, in the above step S3, the heating temperature is 170 ℃, and the thickness of the final composite film product is 0.5-10 mm.
An environment-friendly electromagnetic shielding building material is prepared by any one of the preparation methods of the environment-friendly electromagnetic shielding building material.
In conclusion, the beneficial effects of the invention are as follows:
copper cobaltate nanoparticles are prepared by a hydrothermal method, and excellent electromagnetic wave shielding performance is realized by utilizing the nanometer effect and the electromagnetic property of the copper cobaltate nanoparticles; and is compounded with polyvinylidene fluoride to form a composite membrane material. The composite film can realize better wave-absorbing performance under extremely low composite ratio and thickness, and meanwhile, the film structure can be directly pasted on the inner wall of the existing room to realize a microwave darkroom, so that the use is simple; meanwhile, solvents except alcohol are not used in the preparation process, toxic tail gas is not generated, and byproducts are metal ions which are easy to treat, so that the preparation method has good environmental protection property; under the optimal composite proportion, the maximum absorption of-32 dB can be realized, and the effective working frequency band exceeds 6 GHz.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is an electron micrograph of copper cobaltate nanoparticles according to examples 1 and 2 of the present invention;
FIG. 2 is a graph showing the electromagnetic wave-shielding performance of the composite film of example 1;
fig. 3 is a graph showing the electromagnetic wave shielding performance of the composite film of example 2.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
The invention is illustrated below with reference to fig. 1-3:
example 1
A preparation method of an environment-friendly electromagnetic shielding building material comprises the following steps:
s1, preparing nano copper cobaltate: weighing cobalt nitrate and copper nitrate, mixing with 70% ethanol water solution, stirring to dissolve, adding 30% ammonia water, and adding cetyl trimethyl ammonium bromide. The mixing proportion of the cobalt nitrate, the copper nitrate, the ethanol aqueous solution, the ammonia water and the hexadecyl trimethyl ammonium bromide is as follows: 0.291 g: 0.236 g: 85ml, 5ml and 0.08 g. And stirring the mixture at room temperature for 5 hours, transferring the mixture into a reaction kettle, heating the mixture at 130 ℃ for 500min, centrifuging the mixture and drying the mixture. And (3) burning the dried product at 150 ℃ for 5min in an air atmosphere, and then burning at 400 ℃ for 200min in an argon atmosphere to obtain the copper cobaltate nanoparticles. As shown in fig. 1, an electron micrograph of the copper cobaltate nanoparticles of this example is shown.
S2, preparing a nano copper cobaltate and polyvinylidene fluoride composite film: and (4) mixing 0.1g of the copper cobaltate nanoparticles prepared in the step (S1) and 10g of polyvinylidene fluoride in an acetamide solvent, heating and carrying out ultrasonic treatment, cooling after the mixture is uniform, and drying to obtain the nano copper cobaltate and polyvinylidene fluoride composite membrane.
S3, shaping of a composite film: and (4) heating the nano copper cobaltate and polyvinylidene fluoride composite film prepared in the step (S2) in a mould to 170 ℃, applying certain pressure, and cooling to obtain a final composite film product, wherein the thickness of the composite film is 0.5 mm. As shown in fig. 2, the electromagnetic wave shielding performance of the composite film of the present embodiment is shown as a graph showing the relationship between the reflection loss of the electromagnetic wave and the frequency of the electromagnetic wave.
Example 2
S1, preparing nano copper cobaltate: weighing cobalt nitrate and copper nitrate, mixing with 70% ethanol water solution, stirring to dissolve, adding 30% ammonia water, and adding cetyl trimethyl ammonium bromide. The mixing proportion of the cobalt nitrate, the copper nitrate, the ethanol aqueous solution, the ammonia water and the hexadecyl trimethyl ammonium bromide is as follows: 0.291 g: 0.236 g: 85ml, 5ml and 0.08 g. The mixture was stirred at room temperature for 5 h. Then transferring the mixture into a reaction kettle, heating the mixture for 500min at 130 ℃, centrifuging the mixture and drying the mixture. And (3) burning the dried product at 150 ℃ for 5min in an air atmosphere, and then burning at 400 ℃ for 200min in an argon atmosphere to obtain the copper cobaltate nanoparticles. As shown in fig. 1, an electron micrograph of the copper cobaltate nanoparticles of this example is shown.
S2, preparing a nano copper cobaltate and polyvinylidene fluoride composite film: and (4) mixing 0.1g of nano copper cobaltate prepared in the step (S1) and 10g of polyvinylidene fluoride in an acetamide solvent, heating and carrying out ultrasonic treatment, cooling after the mixture is uniform, and drying to obtain the nano copper cobaltate and polyvinylidene fluoride composite membrane.
S3, shaping of a composite film: and (4) heating the nano copper cobaltate and polyvinylidene fluoride composite film prepared in the step (S2) in a mould to 170 ℃, applying certain pressure, and cooling to obtain a final composite film product, wherein the thickness of the composite film is 0.2 mm. As shown in fig. 3, the electromagnetic wave shielding performance of the composite film of the present embodiment is shown as a graph showing the relationship between the reflection loss of the electromagnetic wave and the frequency of the electromagnetic wave.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103509298A (en) * | 2012-06-20 | 2014-01-15 | 中国科学院合肥物质科学研究院 | Fluoroplastic-based micro-nano composite wave-absorbing material and preparation method thereof |
| CN108659506A (en) * | 2018-05-04 | 2018-10-16 | 南京恒新新材料有限公司 | A kind of nanometer of cuprous sulfide composite electromagnetic shield materials and preparation method thereof |
| RU2705967C1 (en) * | 2018-05-23 | 2019-11-12 | МСД Текнолоджис С.а.р.л. | Screening polymer film and method of its production |
| CN111535044A (en) * | 2020-06-01 | 2020-08-14 | 中国科学院合肥物质科学研究院 | Electromagnetic shielding and hydrophobic functional fabric with high absorption characteristic and preparation method thereof |
| CN111660641A (en) * | 2020-06-24 | 2020-09-15 | 四川大学 | Polymer electromagnetic shielding composite material with multilayer cellular structure and preparation method thereof |
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- 2021-09-29 CN CN202111147870.8A patent/CN113754911B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103509298A (en) * | 2012-06-20 | 2014-01-15 | 中国科学院合肥物质科学研究院 | Fluoroplastic-based micro-nano composite wave-absorbing material and preparation method thereof |
| CN108659506A (en) * | 2018-05-04 | 2018-10-16 | 南京恒新新材料有限公司 | A kind of nanometer of cuprous sulfide composite electromagnetic shield materials and preparation method thereof |
| RU2705967C1 (en) * | 2018-05-23 | 2019-11-12 | МСД Текнолоджис С.а.р.л. | Screening polymer film and method of its production |
| CN111535044A (en) * | 2020-06-01 | 2020-08-14 | 中国科学院合肥物质科学研究院 | Electromagnetic shielding and hydrophobic functional fabric with high absorption characteristic and preparation method thereof |
| CN111660641A (en) * | 2020-06-24 | 2020-09-15 | 四川大学 | Polymer electromagnetic shielding composite material with multilayer cellular structure and preparation method thereof |
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