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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尚晨光
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Shanghai Alede Industrial Group 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

耐候吸波体组合物及其制备方法Weather-resistant wave absorber composition and preparation method thereof

技术领域technical field

本发明涉及材料领域,具体涉及电磁波吸收材料。The invention relates to the field of materials, in particular to electromagnetic wave absorbing materials.

背景技术Background technique

随着信息技术的飞速发展,各种数字化、高频化的电器设备不断向着小型化、数字化和集成化方向发展,设备间通讯复杂度越来越高,很容易受到内部或外部的电磁干扰而出现功能的错误或失效。目前传统的电磁波吸收材料尚不能满足市场的需求,这是因为单一的电磁波吸收材料频带比较杂,无法解决反射问题,因此一般采用透波材料与吸收材料等多元复合组成电磁波吸收体,使得更多的电磁波进入材料内部,而不是从表面反射回去,从而电磁波的吸收效率。一般而言,吸收体的透波材料和吸收材料分开制备,通过层压等方式复合而成,存在着制备工艺比较复杂,难以制备复杂的吸收体等缺点。With the rapid development of information technology, all kinds of digital and high-frequency electrical equipment are constantly developing in the direction of miniaturization, digitization and integration. The communication complexity between devices is getting higher and higher, and they are easily affected by internal or external electromagnetic interference. A functional error or failure has occurred. At present, traditional electromagnetic wave absorbing materials can not meet the needs of the market. This is because a single electromagnetic wave absorbing material has a complex frequency band and cannot solve the reflection problem. Therefore, a multi-component composite such as wave-transmitting material and absorbing material is generally used to form an electromagnetic wave absorber, which makes more The electromagnetic wave enters the material inside, instead of being reflected back from the surface, so the absorption efficiency of electromagnetic wave. Generally speaking, the wave-transmitting material and the absorbing material of the absorber are prepared separately and compounded by lamination, etc., and there are disadvantages such as complicated preparation process and difficulty in preparing complex absorbers.

发明内容SUMMARY OF THE INVENTION

本发明的目的在于提供一种耐候吸波体组合物,以解决上述技术问题。The purpose of the present invention is to provide a weather-resistant wave absorber composition to solve the above-mentioned technical problems.

本发明的目的还在于提供耐候吸波体组合物的制备方法,用于制备耐候吸波体组合物。Another object of the present invention is to provide a preparation method of the weather-resistant wave absorbing body composition for preparing the weather-resistant wave absorbing body composition.

本发明所解决的技术问题可以采用以下技术方案来实现:The technical problem solved by the present invention can be realized by the following technical solutions:

耐候吸波体组合物,其特征在于,包括如下质量百分比的原料:50-90份甲基乙烯基硅树脂、10-50份苯基乙烯基硅树脂、1-10份补强填料、1-10份交联剂、0.002-0.02份铂金催化剂、0.0002-0.004份抑制剂、50-150份磁性吸波剂。本专利对组合物的材质进行了选取,选取后的材料耐候性好,而且允许通过一步法制备。A weather-resistant wave absorber composition, characterized in that it comprises the following raw materials by mass percentage: 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 crosslinking agent, 0.002-0.02 part of platinum catalyst, 0.0002-0.004 part of inhibitor, 50-150 parts of magnetic wave absorber. In this patent, the material of the composition is selected, the selected material has good weather resistance, and can be prepared by a one-step method.

优选,所述甲基乙烯基硅树脂粘度5000-10000mPa·s,乙烯基质量分数0.8-1.6%。所述苯基乙烯基硅树脂粘度3000-10000mPa·s,苯基质量分数10-50%,乙烯基质量分数0.2-0.8%。本专利对选用甲基乙烯基硅树脂和苯基乙烯基硅树脂作为基材,具有优异的耐候性。Preferably, the methyl vinyl silicone resin has a viscosity of 5000-10000 mPa·s and a vinyl mass fraction of 0.8-1.6%. The viscosity of the phenyl vinyl silicone resin is 3000-10000 mPa·s, the mass fraction of phenyl is 10-50%, and the mass fraction of vinyl is 0.2-0.8%. This patent has excellent weather resistance for selecting methyl vinyl silicone resin and phenyl vinyl silicone resin as the base material.

优选,所述补强剂为气相白炭黑或沉淀白炭黑。本专利对补强剂进行了选取,可提高吸波体的力学强度。Preferably, the reinforcing agent is fumed silica or precipitated silica. This patent selects the reinforcing agent, which can improve the mechanical strength of the wave absorber.

所述交联剂为含氢硅油,包括氢质量分数0.6-1.5%侧基含氢硅油和0.05-0.1%端基含氢硅油。所述铂金催化剂包括卡斯特铂金催化剂,铂金含量为3000-5000ppm。所述抑制剂包括1-乙炔-1-环己醇、3-甲基-1-丁炔-3-醇、3,5-二甲基-1-己炔-3-醇、3-苯基-1-丁炔-3-醇中的一种或两种的组合物或两种以上的组合物。所述磁性吸波剂包括铁氧体粉体、羰基铁粉等磁性吸波剂,磁性吸波剂粒径0.05-100微米,形貌包括针状、棒状、片状、球状等,优选棒状或片状吸波剂。The cross-linking agent is hydrogen-containing silicone oil, including 0.6-1.5% hydrogen-containing silicone oil of side groups and 0.05-0.1% hydrogen-containing silicone oil of end groups. The platinum catalyst includes a Custer platinum catalyst, and the platinum content is 3000-5000 ppm. The inhibitors include 1-acetylene-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, 3-phenyl -1-butyn-3-ol in a combination of one or two or a combination of two or more. The magnetic wave absorbing agent includes 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, and the shape includes needle-like, rod-like, flake-like, spherical, etc., preferably rod-like or Sheet absorber.

耐候吸波体组合物的制备方法,其特征在于,将耐候吸波体组合物制备用原料放入混合设备内混合,制得混合物,将混合物装入模具中,向模具施加磁场,使磁性填料向下运动,分为上下两层,然后,在100℃-200℃固化1-2h成型。本专利通过磁场作用吸引磁性吸波剂沿磁场方向运动,可实现组合物的一步法制备,制备工艺简单、制备出的组合物性能可靠稳定。The preparation method of the weather-resistant wave absorber composition is characterized in that, the raw materials for the preparation of the weather-resistant wave absorber composition are put into a mixing device and mixed to prepare a mixture, the mixture is put into a mold, and a magnetic field is applied to the mold to make the magnetic filler Move downward, it is divided into upper and lower layers, and then solidify for 1-2 hours at 100℃-200℃. The patent attracts the magnetic wave absorbing agent to move along the direction of the magnetic field through the action of the magnetic field, and can realize the one-step preparation of the composition, the preparation process is simple, and the prepared composition has reliable and stable performance.

优选,通过行星搅拌机、行星混合机等设备混合。Preferably, it is mixed by a planetary mixer, a planetary mixer or the like.

优选,上层由硅树脂构成透波材料,下层由硅树脂和吸波剂构成吸波材料。Preferably, the upper layer is composed of a wave-transmitting material of silicone resin, and the lower layer is composed of a wave-absorbing material composed of silicone resin and a wave absorbing agent.

具体实施方式Detailed ways

为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面进一步阐述本发明。In order to make the technical means, creative features, achieved objects and effects of the present invention easy to understand and understand, the present invention is further described below.

耐候吸波体组合物,包括如下质量百分比的原料:50-90份甲基乙烯基硅树脂、10-50份苯基乙烯基硅树脂、1-10份补强填料、1-10份交联剂、0.002-0.02份铂金催化剂、0.0002-0.004份抑制剂、50-150份磁性吸波剂。本专利对组合物的材质进行了选取,选取后的材料耐候性好,而且允许通过一步法制备。A weather-resistant wave absorber composition, comprising the following raw materials by mass percentage: 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, 50-150 part of magnetic wave absorbing agent. In this patent, the material of the composition is selected, the selected material has good weather resistance, and can be prepared by a one-step method.

优选,所述甲基乙烯基硅树脂粘度5000-10000mPa·s,乙烯基质量分数0.8-1.6%。所述苯基乙烯基硅树脂粘度3000-10000mPa·s,苯基质量分数10-50%,乙烯基质量分数0.2-0.8%。所述补强剂为气相白炭黑或沉淀白炭黑。本专利对补强剂进行了选取,可提高吸波体的力学强度。所述交联剂为含氢硅油,包括氢质量分数0.6-1.5%侧基含氢硅油和0.05-0.1%端基含氢硅油。所述铂金催化剂包括卡斯特铂金催化剂,铂金含量为3000-5000ppm。所述抑制剂包括1-乙炔-1-环己醇、3-甲基-1-丁炔-3-醇、3,5-二甲基-1-己炔-3-醇、3-苯基-1-丁炔-3-醇中的一种或两种的组合物或两种以上的组合物。所述磁性吸波剂包括铁氧体粉体、羰基铁粉等磁性吸波剂,磁性吸波剂粒径0.05-100微米,形貌包括针状、棒状、片状、球状等,优选棒状或片状吸波剂。Preferably, the methyl vinyl silicone resin has a viscosity of 5000-10000 mPa·s and a vinyl mass fraction of 0.8-1.6%. The viscosity of the phenyl vinyl silicone resin is 3000-10000 mPa·s, the mass fraction of phenyl is 10-50%, and the mass fraction of vinyl is 0.2-0.8%. The reinforcing agent is fumed silica or precipitated silica. This patent selects the reinforcing agent, which can improve the mechanical strength of the wave absorber. The cross-linking agent is hydrogen-containing silicone oil, including 0.6-1.5% hydrogen-containing silicone oil of side groups and 0.05-0.1% hydrogen-containing silicone oil of end groups. The platinum catalyst includes a Custer platinum catalyst, and the platinum content is 3000-5000 ppm. The inhibitors include 1-acetylene-1-cyclohexanol, 3-methyl-1-butyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, 3-phenyl -1-butyn-3-ol in a combination of one or two or a combination of two or more. The magnetic wave absorbing agent includes 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, and the shape includes needle-like, rod-like, flake-like, spherical, etc., preferably rod-like or Flake Absorber.

耐候吸波体组合物的制备方法,将耐候吸波体组合物制备用原料放入混合设备内混合,制得混合物,将混合物装入模具中,向模具施加磁场,使磁性填料向下运动,分为上下两层,然后,在100℃-200℃固化1-2h成型。The preparation method of the weather-resistant wave absorbing body composition comprises the following steps: putting the raw materials for the preparation of the weather-resistant wave absorbing body composition into a mixing device and mixing to obtain a mixture, putting the mixture into a mold, applying a magnetic field to the mold, and causing the magnetic filler to move downward, Divided into upper and lower layers, and then cured for 1-2 hours at 100℃-200℃.

具体实施例1Specific Example 1

原料配比:70份甲基乙烯基硅树脂、30份苯基乙烯基硅树脂、6份疏水性气相白炭黑、4份侧基含氢硅油,2份端基含氢硅油,0.005份铂金催化剂,0.001份1-乙炔-1-环己醇,80份铁氧体粉体。甲基乙烯基硅树脂中乙烯基质量分数1%。苯基乙烯基硅树脂中乙烯基质量分数0.5%,苯基质量分数30%。疏水性气相白炭黑比表面积200g/m2。侧基含氢硅油氢质量分数0.8%,端基含氢硅油氢质量分数0.05%。铂金催化剂铂金质量分数3000ppm。铁氧体粉体粒径10um,片状形貌。Raw material ratio: 70 parts of methyl vinyl silicone resin, 30 parts of phenyl vinyl silicone resin, 6 parts of hydrophobic fumed silica, 4 parts of side-group hydrogen-containing silicone oil, 2 parts of end-group hydrogen-containing silicone oil, 0.005 parts of platinum Catalyst, 0.001 part of 1-acetylene-1-cyclohexanol, 80 parts of ferrite powder. The mass fraction of vinyl in methyl vinyl silicone resin is 1%. The mass fraction of vinyl in the phenyl vinyl silicone resin is 0.5%, and the mass fraction of phenyl is 30%. The specific surface area of hydrophobic fumed silica is 200g/m2. The hydrogen mass fraction of the side group hydrogen-containing silicone oil is 0.8%, and the hydrogen mass fraction of the end group hydrogen-containing silicone oil is 0.05%. Platinum catalyst platinum mass fraction 3000ppm. The ferrite powder has a particle size of 10um and a flake shape.

制备方法:该组合物在30cm*30cm*4mm(长*宽*高)模具中通过磁场作用吸引磁性填料向下移动,分为上下两层,上层由无吸波剂的硅树脂构成透波材料,厚度约2mm;下层由硅树脂和吸波剂构成吸波材料,厚度约2mm,再在100-200℃烘箱中固化1-2h得到吸波体。Preparation method: The composition attracts the magnetic filler to move downward in a 30cm*30cm*4mm (length*width*height) mold through the action of a magnetic field, and is divided into upper and lower layers, and the upper layer is composed of a wave-transmitting material without a wave-absorbing agent , the thickness is about 2mm; the lower layer is composed of silicone resin and wave absorbing agent, the thickness is about 2mm, and then cured in an oven at 100-200 ° C for 1-2 hours to obtain a wave absorbing body.

具体实施例2Specific embodiment 2

原料配比:70份甲基乙烯基硅树脂、30份苯基乙烯基硅树脂、6份疏水性气相白炭黑、4份侧基含氢硅油,2份端基含氢硅油,0.005份铂金催化剂,0.001份1-乙炔-1-环己醇,80份羰基铁粉。甲基乙烯基硅树脂中乙烯基质量分数1%。苯基乙烯基硅树脂中乙烯基质量分数0.5%,苯基质量分数30%。疏水性气相白炭黑比表面积200g/m2。侧基含氢硅油氢质量分数0.8%,端基含氢硅油氢质量分数0.05%。铂金催化剂铂金质量分数3000ppm。羰基铁粉粒径1um,片状形貌。Raw material ratio: 70 parts of methyl vinyl silicone resin, 30 parts of phenyl vinyl silicone resin, 6 parts of hydrophobic fumed silica, 4 parts of side-group hydrogen-containing silicone oil, 2 parts of end-group hydrogen-containing silicone oil, 0.005 parts of platinum Catalyst, 0.001 parts of 1-acetylene-1-cyclohexanol, 80 parts of carbonyl iron powder. The mass fraction of vinyl in methyl vinyl silicone resin is 1%. The mass fraction of vinyl in the phenyl vinyl silicone resin is 0.5%, and the mass fraction of phenyl is 30%. The specific surface area of hydrophobic fumed silica is 200g/m2. The hydrogen mass fraction of the side group hydrogen-containing silicone oil is 0.8%, and the hydrogen mass fraction of the end group hydrogen-containing silicone oil is 0.05%. Platinum catalyst platinum mass fraction 3000ppm. The carbonyl iron powder has a particle size of 1um and a flake shape.

制备方法:该组合物在30cm*30cm*4mm(长*宽*高)模具中通过磁场作用吸引磁性填料向下移动,分为上下两层,上层由无吸波剂的硅树脂构成透波材料,厚度约1mm;下层由硅树脂和吸波剂构成吸波材料,厚度约3mm,再在100-200℃烘箱中固化1-2h得到吸波体。Preparation method: The composition attracts the magnetic filler to move downward in a 30cm*30cm*4mm (length*width*height) mold through the action of a magnetic field, and is divided into upper and lower layers, and the upper layer is composed of a wave-transmitting material without a wave-absorbing agent , the thickness is about 1mm; the lower layer is composed of silicone resin and wave absorbing agent, the thickness is about 3mm, and then cured in an oven at 100-200 ° C for 1-2 hours to obtain a wave absorbing body.

对比例一Comparative Example 1

与具体实施例1相同的配方,不同的是对比例1中不加入气相白炭黑。The formula is the same as that of the specific example 1, except that the fumed silica is not added in the comparative example 1.

对比例二Comparative Example 2

与具体实施例2相同的配方,不同的是通过加大磁场,得到透波材料厚度约3mm,而吸波材料1mm的吸波体。The same formula as the specific embodiment 2, the difference is that by increasing the magnetic field, a wave-absorbing body with a thickness of about 3 mm of the wave-transmitting material and 1 mm of the wave-absorbing material is obtained.

分别对具体实施例1、具体实施例2和对比例一、对比例二成型组合物进行测试,基于GB/T 528对拉伸强度进行测试,基于GJB 2038-1994对吸波体反射率测试,测试结果如表一所示。The specific embodiment 1, the specific embodiment 2 and the comparative example 1 and the comparative example 2 are tested respectively, the tensile strength is tested based on GB/T 528, and the reflectivity of the wave absorber is tested based on GJB 2038-1994, The test results are shown in Table 1.

Figure BDA0002812509240000041
Figure BDA0002812509240000041

根据测试结果可以看出:According to the test results, it can be seen that:

1.具体实施例2制备出的组合物的性能非常优异。1. The performance of the composition prepared in specific example 2 is very excellent.

2.气相白炭黑的添加具有非常好的效果。2. The addition of fumed silica has a very good effect.

需要说明的是,在本文中,诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。It should be noted that, in this document, relational terms such as first and second are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any relationship between these entities or operations. any such actual relationship or sequence exists. Moreover, the terms "comprising", "comprising" or any other variation thereof are intended to encompass non-exclusive inclusion such that a process, method, article or device comprising a list of elements includes not only those elements, but also includes not explicitly listed or other elements inherent to such a process, method, article or apparatus. Without further limitation, an element qualified by the phrase "comprising a..." does not preclude the presence of additional identical elements in a process, method, article or apparatus that includes the element.

以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。The foregoing has shown and described the basic principles and main features of the present invention, as well as the advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above-mentioned embodiments. The above-mentioned embodiments and descriptions only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Various changes and modifications fall within the scope of the claimed invention. The claimed scope of the present invention is defined by the appended claims and their equivalents.

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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