CN112662183B - Weather-resistant wave absorber composition and preparation method thereof - Google Patents

Weather-resistant wave absorber composition and preparation method thereof Download PDF

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CN112662183B
CN112662183B CN202011393271.XA CN202011393271A CN112662183B CN 112662183 B CN112662183 B CN 112662183B CN 202011393271 A CN202011393271 A CN 202011393271A CN 112662183 B CN112662183 B CN 112662183B
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wave absorber
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CN112662183A (en
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尚晨光
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Shanghai Allied Industrial Co ltd
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Abstract

A weather-resistant wave absorber composition and a preparation method thereof relate to the field of materials. The weather-resistant wave absorber composition is characterized by comprising the following raw materials in percentage by mass: 50-90 parts of methyl vinyl silicone resin, 10-50 parts of phenyl vinyl silicone resin, 1-10 parts of reinforcing filler, 1-10 parts of cross-linking agent, 0.002-0.02 part of platinum catalyst, 0.0002-0.004 part of inhibitor and 50-150 parts of magnetic wave absorbing agent. The patent selects the material of the composition, the selected material has good weather resistance, and the composition can be prepared by a one-step method. The preparation method of the weather-resistant wave absorber composition is used for preparing the weather-resistant wave absorber composition.

Description

Weather-resistant wave absorber composition and preparation method thereof
Technical Field
The invention relates to the field of materials, in particular to an electromagnetic wave absorbing material.
Background
With the rapid development of information technology, various digital and high-frequency electrical devices are continuously developed towards miniaturization, digitalization and integration, and the complexity of communication between devices is higher and higher, so that the devices are easily subjected to internal or external electromagnetic interference to cause functional errors or failures. At present, the traditional electromagnetic wave absorbing material cannot meet the market demand, because the single electromagnetic wave absorbing material has a relatively complicated frequency band and cannot solve the reflection problem, the electromagnetic wave absorbing body is generally formed by compounding multiple elements such as a wave-transmitting material, an absorbing material and the like, so that more electromagnetic waves enter the material instead of being reflected from the surface, and the absorption efficiency of the electromagnetic waves is further improved. In general, a wave-transmitting material and an absorbing material of an absorber are separately prepared and combined by lamination or the like, and there are disadvantages that the preparation process is complicated and it is difficult to prepare a complicated absorber.
Disclosure of Invention
The invention aims to provide a weather-resistant wave absorber composition to solve the technical problems.
The invention also aims to provide a preparation method of the weather-resistant wave absorber composition, which is used for preparing the weather-resistant wave absorber composition.
The technical problem solved by the invention can be realized by adopting the following technical scheme:
the weather-resistant wave absorber composition is characterized by comprising the following raw materials in percentage by mass: 50-90 parts of methyl vinyl silicone resin, 10-50 parts of phenyl vinyl silicone resin, 1-10 parts of reinforcing filler, 1-10 parts of cross-linking agent, 0.002-0.02 part of platinum catalyst, 0.0002-0.004 part of inhibitor and 50-150 parts of magnetic wave absorbing agent. The patent selects the material of the composition, the selected material has good weather resistance, and the composition can be prepared by a one-step method.
Preferably, the viscosity of the methyl vinyl silicone resin is 5000-10000mPa & s, and the vinyl mass fraction is 0.8-1.6%. The viscosity of the phenyl vinyl silicone resin is 3000-10000mPa & s, the mass fraction of the phenyl is 10-50%, and the mass fraction of the vinyl is 0.2-0.8%. This patent is to selecting methyl vinyl silicone resin and phenyl vinyl silicone resin as the substrate, has excellent weatherability.
Preferably, the reinforcing agent is fumed silica or precipitated silica. This patent has carried out the selection to the reinforcing agent, can improve the mechanical strength of wave absorber.
The cross-linking agent is hydrogen-containing silicone oil, and comprises 0.6-1.5% of lateral group hydrogen-containing silicone oil and 0.05-0.1% of terminal group hydrogen-containing silicone oil in terms of hydrogen mass fraction. The platinum catalyst comprises a Kanst platinum catalyst, and the platinum content is 3000-5000 ppm. The inhibitor comprises one or a composition of two or more of 1-acetylene-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol and 3-phenyl-1-butyn-3-ol. The magnetic wave absorbing agent comprises ferrite powder, carbonyl iron powder and other magnetic wave absorbing agents, the particle size of the magnetic wave absorbing agent is 0.05-100 microns, the appearance of the magnetic wave absorbing agent comprises needle-shaped, rod-shaped, sheet-shaped, spherical and the like, and the rod-shaped or sheet-shaped wave absorbing agent is preferred.
The preparation method of the weather-resistant wave absorber composition is characterized in that raw materials for preparing the weather-resistant wave absorber composition are placed into a mixing device to be mixed to prepare a mixture, the mixture is placed into a mold, a magnetic field is applied to the mold to enable a magnetic filler to move downwards and to be divided into an upper layer and a lower layer, and then the mixture is cured for 1-2 hours at the temperature of 100-200 ℃ to be molded. The magnetic wave absorber is attracted to move along the magnetic field direction under the action of the magnetic field, so that the one-step preparation of the composition can be realized, the preparation process is simple, and the prepared composition has reliable and stable performance.
Preferably, the mixing is carried out by means of a planetary mixer, a planetary mixer or the like.
Preferably, the upper layer is made of silicon resin to form a wave-transmitting material, and the lower layer is made of silicon resin and a wave-absorbing agent to form a wave-absorbing material.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further explained below.
The weather-resistant wave absorber composition comprises the following raw materials in percentage by mass: 50-90 parts of methyl vinyl silicone resin, 10-50 parts of phenyl vinyl silicone resin, 1-10 parts of reinforcing filler, 1-10 parts of cross-linking agent, 0.002-0.02 part of platinum catalyst, 0.0002-0.004 part of inhibitor and 50-150 parts of magnetic wave absorbing agent. The composite material is selected, has good weather resistance and can be prepared by a one-step method.
Preferably, the viscosity of the methyl vinyl silicone resin is 5000-10000mPa & s, and the vinyl mass fraction is 0.8-1.6%. The viscosity of the phenyl vinyl silicone resin is 3000-10000mPa & s, the mass fraction of the phenyl is 10-50%, and the mass fraction of the vinyl is 0.2-0.8%. The reinforcing agent is fumed silica or precipitated silica. This patent has carried out the selection to the reinforcing agent, can improve the mechanical strength of wave absorber. The cross-linking agent is hydrogen-containing silicone oil, and comprises 0.6-1.5% of lateral group hydrogen-containing silicone oil and 0.05-0.1% of terminal group hydrogen-containing silicone oil in terms of hydrogen mass fraction. The platinum catalyst comprises a Kanst platinum catalyst, and the platinum content is 3000-5000 ppm. The inhibitor comprises one or a composition of two or more of 1-acetylene-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol and 3-phenyl-1-butyn-3-ol. The magnetic wave absorbing agent comprises ferrite powder, carbonyl iron powder and other magnetic wave absorbing agents, the particle size of the magnetic wave absorbing agent is 0.05-100 microns, the appearance of the magnetic wave absorbing agent comprises needle-shaped, rod-shaped, sheet-shaped, spherical and the like, and the rod-shaped or sheet-shaped wave absorbing agent is preferred.
The preparation method of the weather-resistant wave absorber composition comprises the steps of putting raw materials for preparing the weather-resistant wave absorber composition into a mixing device for mixing to obtain a mixture, putting the mixture into a mold, applying a magnetic field to the mold to enable a magnetic filler to move downwards to be divided into an upper layer and a lower layer, and then curing at 100-200 ℃ for 1-2 hours for molding.
Detailed description of the preferred embodiment 1
The raw material ratio is as follows: 70 parts of methyl vinyl silicone resin, 30 parts of phenyl vinyl silicone resin, 6 parts of hydrophobic fumed silica, 4 parts of lateral group hydrogen-containing silicone oil, 2 parts of terminal group hydrogen-containing silicone oil, 0.005 part of platinum catalyst, 0.001 part of 1-acetylene-1-cyclohexanol and 80 parts of ferrite powder. The mass fraction of vinyl in the methyl vinyl silicone resin is 1 percent. The mass fraction of vinyl in the phenyl vinyl silicone resin is 0.5 percent, and the mass fraction of phenyl is 30 percent. The specific surface area of the hydrophobic fumed silica is 200g/m 2. The hydrogen mass fraction of the side group hydrogen-containing silicone oil is 0.8 percent, and the hydrogen mass fraction of the end group hydrogen-containing silicone oil is 0.05 percent. The platinum catalyst has a platinum mass fraction of 3000 ppm. The ferrite powder has the particle size of 10um and the shape of a sheet.
The preparation method comprises the following steps: the composition attracts the magnetic filler to move downwards through the action of a magnetic field in a 30 cm-4 mm (length-width-height) die, and the composition is divided into an upper layer and a lower layer, wherein the upper layer is made of a wave-transmitting material consisting of silicone resin without a wave-absorbing agent and has the thickness of about 2 mm; the lower layer is made of silicon resin and wave absorbing agent, the thickness of the wave absorbing material is about 2mm, and the wave absorbing material is cured in an oven at the temperature of 100 ℃ and 200 ℃ for 1-2h to obtain the wave absorbing body.
Specific example 2
The raw material ratio is as follows: 70 parts of methyl vinyl silicone resin, 30 parts of phenyl vinyl silicone resin, 6 parts of hydrophobic fumed silica, 4 parts of lateral group hydrogen-containing silicone oil, 2 parts of terminal group hydrogen-containing silicone oil, 0.005 part of platinum catalyst, 0.001 part of 1-acetylene-1-cyclohexanol and 80 parts of carbonyl iron powder. The mass fraction of vinyl in the methyl vinyl silicone resin is 1 percent. The mass fraction of vinyl in the phenyl vinyl silicone resin is 0.5 percent, and the mass fraction of phenyl is 30 percent. The specific surface area of the hydrophobic fumed silica is 200g/m 2. The hydrogen mass fraction of the side group hydrogen-containing silicone oil is 0.8 percent, and the hydrogen mass fraction of the end group hydrogen-containing silicone oil is 0.05 percent. The mass fraction of platinum in the platinum catalyst is 3000 ppm. The particle size of the carbonyl iron powder is 1um, and the shape of the carbonyl iron powder is flaky.
The preparation method comprises the following steps: the composition attracts the magnetic filler to move downwards through the action of a magnetic field in a 30 cm-4 mm (length-width-height) die, and the composition is divided into an upper layer and a lower layer, wherein the upper layer is made of a wave-transmitting material consisting of silicone resin without a wave-absorbing agent and has the thickness of about 1 mm; the lower layer is made of silicon resin and wave absorbing agent, the thickness of the wave absorbing material is about 3mm, and the wave absorbing material is cured in an oven at the temperature of 100 ℃ and 200 ℃ for 1-2h to obtain the wave absorbing body.
Comparative example 1
The same formulation as in example 1, except that fumed silica was not added in comparative example 1.
Comparative example No. two
The same formula as that of the specific example 2, except that the wave-absorbing body with the thickness of the wave-transmitting material of about 3mm and the wave-absorbing material of 1mm is obtained by increasing the magnetic field.
The molding compositions of the embodiment 1 and the embodiment 2 and the first and the second comparative examples were tested, respectively, the tensile strength was tested based on GB/T528, the wave absorber reflectivity was tested based on GJB 2038-.
Figure BDA0002812509240000041
According to the test results, it can be seen that:
1. the composition prepared in example 2 is very excellent in properties.
2. The addition of fumed silica has a very good effect.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in the process, method, article, or apparatus that comprises the element.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. The weather-resistant wave absorber composition is characterized by comprising the following raw materials: 50-90 parts of methyl vinyl silicone resin, 10-50 parts of phenyl vinyl silicone resin, 1-10 parts of reinforcing filler, 1-10 parts of cross-linking agent, 0.002-0.02 part of platinum catalyst, 0.0002-0.004 part of inhibitor and 50-150 parts of magnetic wave absorbing agent;
putting the raw materials into mixing equipment for mixing to obtain a mixture, putting the mixture into a mould, applying a magnetic field to the mould to enable the magnetic wave absorbing agent to move downwards to be divided into an upper layer and a lower layer, and then curing at 100-200 ℃ for 1-2h for forming;
the upper layer is made of wave-transmitting material without wave-absorbing agent and is 1mm thick; the lower layer is made of wave-absorbing material consisting of silicone resin and wave-absorbing agent, and the thickness of the wave-absorbing material is 3 mm.
2. The weather-resistant wave absorber composition as claimed in claim 1, wherein the methyl vinyl silicone resin has a viscosity of 5000-10000 mPa-s and a vinyl mass fraction of 0.8-1.6%.
3. The weather-resistant wave absorber composition as claimed in claim 1, wherein the viscosity of the phenyl vinyl silicone resin is 3000-10000 mPa-s, the mass fraction of the phenyl is 10-50%, and the mass fraction of the vinyl is 0.2-0.8%.
4. The weather-resistant absorber composition of claim 1, wherein the reinforcing filler is fumed silica or precipitated silica.
5. The composition of claim 1, wherein the crosslinking agent is a hydrogen-containing silicone oil comprising 0.6-1.5% by weight of hydrogen of a pendant hydrogen-containing silicone oil and 0.05-0.1% by weight of a terminal hydrogen-containing silicone oil.
6. The weather-resistant wave absorber composition as claimed in claim 1, wherein the platinum catalyst comprises a Kansted platinum catalyst, and the platinum content is 3000-5000 ppm.
7. The weather-resistant wave absorber composition according to claim 1, wherein the inhibitor comprises one or a combination of two or a combination of more than two of 1-ethyne-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, and 3-phenyl-1-butyn-3-ol.
8. The weather-resistant wave absorber composition of claim 1, wherein the magnetic wave absorber has a particle size of 0.05-100 microns.
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