CN111040453A - Silicone rubber-based wave-absorbing patch and preparation method thereof - Google Patents

Silicone rubber-based wave-absorbing patch and preparation method thereof Download PDF

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Publication number
CN111040453A
CN111040453A CN201911269031.6A CN201911269031A CN111040453A CN 111040453 A CN111040453 A CN 111040453A CN 201911269031 A CN201911269031 A CN 201911269031A CN 111040453 A CN111040453 A CN 111040453A
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absorbing patch
silicone rubber
wave
based wave
magnetic absorbent
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张行
韦国科
尹贻超
高路
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
AVIC Manufacturing Technology Institute
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AVIC Beijing Aeronautical Manufacturing Technology Research Institute
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/01Magnetic additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to the technical field of wave-absorbing patches and provides a silicon rubber-based wave-absorbing patch and a preparation method thereof. The silicon rubber wave-absorbing patch and the novel preparation method thereof are developed, high filling ratio preparation of the silicon rubber wave-absorbing patch with good mechanical property is realized based on surface treatment of the flaky absorbent and addition of organic silicon resin and the like, and the preparation of a high-performance wave-absorbing patch material can be realized; aiming at the problems of low filling ratio and difficult molding of the absorbent in the silicone rubber, the problem of dispersion uniformity is solved by surface treatment of the flaky magnetic absorbent, and the filling ratio is improved; filling a magnetic absorbent, silicon rubber, white carbon black, silicon resin, a vulcanizing agent and the like according to a certain proportion, mixing, uniformly mixing, and performing hot pressing to prepare the wave-absorbing patch; the thickness of the obtained silicon rubber-based wave-absorbing patch is 0.2-3mm, the filling proportion of the magnetic absorbent is more than or equal to 80%, and the elongation at break is more than or equal to 100%.

Description

Silicone rubber-based wave-absorbing patch and preparation method thereof
Technical Field
The invention relates to the technical field of wave-absorbing patches, in particular to a silicon rubber-based wave-absorbing patch and a preparation method thereof.
Background
With the development of aviation stealth weaponry, the requirements for maintenance and replacement of stealth materials of weaponry are higher and higher, and the requirements can be met by adopting a wave-absorbing patch method. At present, the stealth part of the aviation weapon equipment has multiple curvatures, multiple structures and easy damage of partial positions, and the wave-absorbing coating spraying method adopted by the method can cause the problems of difficult construction, longer construction period, repeated later maintenance, high maintenance cost and the like. Compared with the traditional spraying wave-absorbing coating, the wave-absorbing patch material has the advantages of being prepared in advance, adjustable in thickness, capable of detecting the performance in advance, convenient to transport and store and the like, so that the application range of the wave-absorbing patch is widened, and the stealth performance of weapon equipment is improved.
The wave-absorbing patch also has high requirements on the aspects of thinness, width, lightness, strength and the like, and adopts a sheet-shaped absorbent with high wave-absorbing performance and a mode of high filling concentration to realize the wave-absorbing performance under thinner thickness; in order to improve the better temperature resistance and tensile property of the wave-absorbing patch, the silicon rubber is used as a matrix to prepare the wave-absorbing patch.
However, the preparation of the current silicon rubber type wave-absorbing patch mainly has two technical problems: first, the magnetic absorbent filling ratio is difficult to increase; secondly, the mechanical properties of the patch are poor. At present, the dispersion effect of the magnetic absorbent is improved and the filling proportion is increased mainly by adding an organic solvent. However, firstly, the volatilization of the organic solvent easily causes problems such as environmental pollution, and secondly, the too high filling concentration of the magnetic absorbent causes problems such as the reduction of the tensile strength of the rubber patch material and the poor mechanical properties.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a silicon rubber-based wave-absorbing patch; the invention also aims to provide a preparation method of the silicon rubber-based wave-absorbing patch. The compatibility of the magnetic absorbent is improved through the surface modification of the magnetic absorbent; meanwhile, the organic silicon resin is added, so that the dispersion effect of the absorbent is improved, the tackifying property is given to the organic silicon rubber, the mechanical property of the wave-absorbing patch is improved, and the problems of environmental pollution caused by the addition of an organic solvent and the like are solved.
The invention adopts the following technical scheme:
a silicon rubber-based wave-absorbing patch comprises, by weight, 1000 parts of modified flaky magnetic absorbent 800-5 parts of silicon rubber, 100 parts of silica rubber, 1-5 parts of white carbon black, 2-10 parts of organic silicon resin and 2-5 parts of vulcanizing agent.
Preferably, the modified flaky magnetic absorbent is prepared by modifying the surface of a flaky magnetic absorbent through a silane coupling agent.
Preferably, the silane coupling agent is KH550, KH560 and/or KH 570.
Preferably, the modified flaky magnetic absorbent is modified flaky carbonyl iron powder, modified flaky ferrosilicon aluminum powder, modified flaky iron-cobalt nickel powder or modified flaky iron-nickel powder.
Preferably, the silicone rubber is methyl vinyl silicone rubber or methyl phenyl vinyl silicone rubber.
Preferably, the thickness of the silicon rubber-based wave-absorbing patch is 0.2-3 mm.
A preparation method of a silicone rubber-based wave-absorbing patch comprises the following steps:
step one, selecting a sheet-shaped magnetic absorbent with the size of 1-50 microns, adding the sheet-shaped magnetic absorbent into an ethanol solution of a silane coupling agent with the mass concentration of 5%, heating the mixture to 70 ℃ under the condition of mechanical stirring, reacting for 8 hours, washing the mixture with ethanol, and drying the mixture to obtain a surface-modified sheet-shaped magnetic absorbent, namely a modified sheet-shaped magnetic absorbent;
secondly, adding raw silicon rubber on an open mill according to the raw material proportion, then adding white carbon black for reinforcement, continuously mixing, then gradually adding the modified flaky magnetic absorbent and the organic silicon resin, and finally gradually adding the vulcanizing agent for continuous mixing;
thirdly, putting the prepared rubber sheet into a die cavity, and pressing into a die;
and step four, obtaining the silicon rubber-based wave-absorbing patch through hot-pressing treatment and demoulding.
Preferably, in the first step, the mass ratio of the flaky magnetic absorbent to the silane coupling agent is 100: 1.
preferably, in step three, the size of the die cavity is 200mm by 0.5 mm.
Preferably, in the fourth step, the hot pressing treatment is carried out under the conditions of 110-150 ℃ and 15-25MPa for 5-30 min.
The invention has the beneficial effects that:
the silicon rubber wave-absorbing patch is developed and a novel preparation method thereof, high filling ratio preparation of the silicon rubber wave-absorbing patch with good mechanical property is realized based on surface treatment of a flaky absorbent, addition of organic silicon resin and the like, and the preparation of a high-performance wave-absorbing patch material can be realized; aiming at the problems of low filling ratio and difficult molding of the absorbent in the silicone rubber, the problem of dispersion uniformity is solved by surface treatment of the flaky magnetic absorbent, and the filling ratio is improved; filling a magnetic absorbent, silicon rubber, white carbon black, silicon resin, a vulcanizing agent and the like according to a certain proportion, mixing, uniformly mixing, and performing hot pressing to prepare the wave-absorbing patch; the thickness of the obtained silicon rubber-based wave-absorbing patch is 0.2-3mm, the filling proportion of the magnetic absorbent is more than or equal to 80%, and the elongation at break is more than or equal to 100%.
Drawings
FIG. 1 is a SEM (scanning electron microscope) image of the cross section of a silicone rubber-based wave-absorbing patch.
Detailed Description
The present invention will be described in detail with reference to the following examples:
example 1
Test materials: 800 parts of modified flaky carbonyl iron powder, 100 parts of methyl vinyl silicone rubber, 1 part of white carbon black, 2 parts of organic silicon resin and 2 parts of vulcanizing agent.
The method comprises the following specific implementation steps:
step one, selecting a sheet-shaped magnetic absorbent with the size of 1 mu m, adding the sheet-shaped magnetic absorbent into an ethanol solution of a silane coupling agent (KH570) with the mass concentration of 5%, heating the mixture to 70 ℃ under the condition of mechanical stirring, reacting for 8 hours, washing the mixture with ethanol, and drying the mixture to obtain a surface-modified sheet-shaped magnetic absorbent, namely a modified sheet-shaped magnetic absorbent;
secondly, adding raw silicon rubber on an open mill according to the raw material proportion, then adding white carbon black for reinforcement, continuously mixing, then gradually adding the modified flaky magnetic absorbent and the organic silicon resin, and finally gradually adding the vulcanizing agent for continuous mixing;
thirdly, putting the prepared rubber sheet into a die cavity, pressing the rubber sheet into a die with the size of 200mm to 0.5 mm;
and step four, hot pressing for 30min at the temperature of 110 ℃ and under the pressure of 15MPa, and demolding to obtain the silicon rubber-based wave-absorbing patch.
Through detection, the thickness of the silicon rubber-based wave-absorbing patch is 0.2mm, the filling proportion of the magnetic absorbent is more than or equal to 80 percent, and the elongation at break is more than or equal to 100 percent. The SEM image of the cross section is shown in FIG. 1.
Example 2
Test materials: 1000 parts of modified flaky ferrosilicon aluminum powder, 100 parts of methyl phenyl vinyl silicone rubber, 5 parts of white carbon black, 10 parts of organic silicon resin and 5 parts of vulcanizing agent.
The method comprises the following specific implementation steps:
step one, selecting a 50-micron sheet-shaped magnetic absorbent, adding the sheet-shaped magnetic absorbent into an ethanol solution of a silane coupling agent (KH560 and KH570) with the mass concentration of 5%, heating the mixture to 70 ℃ under the condition of mechanical stirring, reacting for 8 hours, washing the mixture with ethanol, and drying the mixture to obtain a surface-modified sheet-shaped magnetic absorbent, namely a modified sheet-shaped magnetic absorbent;
secondly, adding raw silicon rubber on an open mill according to the raw material proportion, then adding white carbon black for reinforcement, continuously mixing, then gradually adding the modified flaky magnetic absorbent and the organic silicon resin, and finally gradually adding the vulcanizing agent for continuous mixing;
thirdly, putting the prepared rubber sheet into a die cavity, pressing the rubber sheet into a die with the size of 200mm to 0.5 mm;
and step four, hot pressing for 5min at 150 ℃ and 25MPa, and demolding to obtain the silicon rubber-based wave-absorbing patch.
Example 3
Test materials: according to the weight portion, 800 portions of modified flaky carbonyl iron powder and 1000 portions of modified flaky carbonyl iron powder, 100 portions of methyl vinyl silicone rubber, 1 to 5 portions of white carbon black, 2 to 10 portions of organic silicon resin and 2 to 5 portions of vulcanizing agent.
The specific implementation steps are as follows:
step one, selecting a sheet-shaped magnetic absorbent with the size of 1-50 microns, adding the sheet-shaped magnetic absorbent into an ethanol solution containing a silane coupling agent (KH550) with the mass fraction of 5%, heating the mixture to 70 ℃ under the condition of mechanical stirring, reacting for 8 hours, and washing and drying the ethanol to obtain a surface-modified sheet-shaped magnetic absorbent;
secondly, adding raw silicon rubber on an open mill according to the raw material proportion, then adding white carbon black for reinforcement, continuously mixing, then gradually adding the surface-modified flaky magnetic absorbent and the organic silicon resin, and finally gradually adding the vulcanizing agent for continuous mixing;
putting the prepared film into a die cavity with the size of about 200mm by 0.5mm, and pressing the film into a die;
and step four, hot pressing for 5-30min at the temperature of 110-150 ℃ and under the pressure of 15-25MPa, and demolding to obtain the rubber patch.
Example 4
Test materials: according to weight portion, 100 portions of methyl phenyl vinyl silicone rubber, 1000 portions of modified flaky carbonyl iron powder 800-one, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
The procedure was the same as in example 1.
Example 5
Test materials: according to the weight portion, 100 portions of methyl vinyl silicone rubber, 1000 portions of modified flaky ferrosilicon aluminum powder 800-one, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
The procedure was the same as in example 1.
Example 6
Test materials: according to weight portion, 100 portions of methyl vinyl silicone rubber, 1000 portions of modified flaky iron-cobalt nickel powder 800-one, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
The procedure was the same as in example 1.
Example 7
Test materials: according to weight portion, 100 portions of methyl vinyl silicone rubber, 1000 portions of 800-sand modified flaky iron nickel powder, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
The procedure was the same as in example 1.
Example 8
Test materials: according to weight portion, 100 portions of methyl phenyl vinyl silicone rubber, 1000 portions of 800-iron nickel powder, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
The procedure was the same as in example 1.
Example 9
Test materials: according to weight portion, 100 portions of methyl phenyl vinyl silicone rubber, 1000 portions of modified flaky carbonyl iron powder 800-one, 1-5 portions of white carbon black, 2-10 portions of organic silicon resin and 2-5 portions of vulcanizing agent.
In the first step, the silane coupling agents KH560 and KH570 were surface-treated, and the other steps were the same as in example 1.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art may make modifications, alterations, additions or substitutions within the spirit and scope of the present invention.

Claims (10)

1. A silicon rubber-based wave-absorbing patch is characterized by comprising, by weight, 1000 parts of modified flaky magnetic absorbent 800-1000 parts, 100 parts of silicon rubber, 1-5 parts of white carbon black, 2-10 parts of organic silicon resin and 2-5 parts of vulcanizing agent.
2. The silicone rubber-based wave-absorbing patch according to claim 1, wherein the modified sheet-like magnetic absorbent is prepared by modifying the surface of a sheet-like magnetic absorbent with a silane coupling agent.
3. The silicone rubber-based wave absorbing patch as claimed in claim 2, wherein the silane coupling agent is KH550, KH560 and/or KH 570.
4. The silicone rubber-based wave-absorbing patch according to claim 1, wherein the modified flaky magnetic absorbent is modified flaky carbonyl iron powder, modified flaky ferrosilicon aluminum powder, modified flaky iron-cobalt nickel powder or modified flaky iron-nickel powder.
5. The silicone rubber-based wave absorbing patch according to claim 1, wherein the silicone rubber is methyl vinyl silicone rubber or methyl phenyl vinyl silicone rubber.
6. The silicone rubber-based wave-absorbing patch according to claim 1, wherein the silicone rubber-based wave-absorbing patch has a thickness of 0.2-3 mm.
7. A preparation method of a silicon rubber-based wave-absorbing patch is characterized by comprising the following steps:
step one, selecting a sheet-shaped magnetic absorbent with the size of 1-50 microns, adding the sheet-shaped magnetic absorbent into an ethanol solution of a silane coupling agent with the mass concentration of 5%, heating the mixture to 70 ℃ under the condition of mechanical stirring, reacting for 8 hours, washing the mixture with ethanol, and drying the mixture to obtain a surface-modified sheet-shaped magnetic absorbent, namely a modified sheet-shaped magnetic absorbent;
secondly, adding raw silicon rubber on an open mill according to the raw material proportion, then adding white carbon black for reinforcement, continuously mixing, then gradually adding the modified flaky magnetic absorbent and the organic silicon resin, and finally gradually adding the vulcanizing agent for continuous mixing;
thirdly, putting the prepared rubber sheet into a die cavity, and pressing into a die;
and step four, obtaining the silicon rubber-based wave-absorbing patch through hot-pressing treatment and demoulding.
8. The preparation method of the silicone rubber-based wave-absorbing patch according to claim 7, wherein in the first step, the mass ratio of the sheet-shaped magnetic absorbent to the silane coupling agent is 100: 1.
9. the method for preparing the silicone rubber-based wave-absorbing patch according to claim 7, wherein in the third step, the size of the mold cavity is 200mm by 0.5 mm.
10. The method for preparing a silicone rubber-based wave-absorbing patch as claimed in claim 7, wherein in the fourth step, the hot pressing treatment is performed under the conditions of 110-150 ℃ and 15-25MPa for 5-30 min.
CN201911269031.6A 2019-12-11 2019-12-11 Silicone rubber-based wave-absorbing patch and preparation method thereof Pending CN111040453A (en)

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CN112980398A (en) * 2021-02-24 2021-06-18 天津泽希新材料有限公司 High-thermal-conductivity wave-absorbing silica gel gasket and preparation method thereof
CN113583497A (en) * 2021-08-09 2021-11-02 中国航空制造技术研究院 Preparation method of thickness-insensitive double-layer wave-absorbing coating material
CN114634712A (en) * 2020-12-15 2022-06-17 洛阳尖端技术研究院 Wave-absorbing rubber, preparation method thereof and wave-absorbing device
CN114891353A (en) * 2022-06-28 2022-08-12 北京科技大学广州新材料研究院 Composite gasket, preparation method and application thereof, and electronic device
CN114957995A (en) * 2022-05-17 2022-08-30 北京科技大学广州新材料研究院 Corrosion-resistant wave-absorbing heat-conducting silicone rubber composite gasket and preparation method thereof
CN115109418A (en) * 2022-08-01 2022-09-27 航天科工武汉磁电有限责任公司 Wave-absorbing silicone rubber and preparation method thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114634712A (en) * 2020-12-15 2022-06-17 洛阳尖端技术研究院 Wave-absorbing rubber, preparation method thereof and wave-absorbing device
CN112980398A (en) * 2021-02-24 2021-06-18 天津泽希新材料有限公司 High-thermal-conductivity wave-absorbing silica gel gasket and preparation method thereof
CN113583497A (en) * 2021-08-09 2021-11-02 中国航空制造技术研究院 Preparation method of thickness-insensitive double-layer wave-absorbing coating material
CN113583497B (en) * 2021-08-09 2022-02-15 中国航空制造技术研究院 Preparation method of thickness-insensitive double-layer wave-absorbing coating material
CN114957995A (en) * 2022-05-17 2022-08-30 北京科技大学广州新材料研究院 Corrosion-resistant wave-absorbing heat-conducting silicone rubber composite gasket and preparation method thereof
CN114957995B (en) * 2022-05-17 2024-01-02 北京科技大学广州新材料研究院 Corrosion-resistant wave-absorbing heat-conducting silicon rubber composite gasket and preparation method thereof
CN114891353A (en) * 2022-06-28 2022-08-12 北京科技大学广州新材料研究院 Composite gasket, preparation method and application thereof, and electronic device
CN114891353B (en) * 2022-06-28 2023-11-03 北京科技大学广州新材料研究院 Composite gasket, preparation method and application thereof, and electronic device
CN115109418A (en) * 2022-08-01 2022-09-27 航天科工武汉磁电有限责任公司 Wave-absorbing silicone rubber and preparation method thereof

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