CN108864839A - 一种膨胀石墨阻燃灭火材料及其制备方法 - Google Patents

一种膨胀石墨阻燃灭火材料及其制备方法 Download PDF

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CN108864839A
CN108864839A CN201710335947.1A CN201710335947A CN108864839A CN 108864839 A CN108864839 A CN 108864839A CN 201710335947 A CN201710335947 A CN 201710335947A CN 108864839 A CN108864839 A CN 108864839A
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expanded graphite
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张立强
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Have New Materials (huizhou) Co Ltd
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Abstract

本发明公开了一种膨胀石墨阻燃灭火材料及其制作方法，包括以下重量份的组分：有机树脂5～40份、膨胀石墨粉0.5～30份、导热导电粉体10～80份、偶联剂1～10份、固化剂0.5～5份及助剂0.5～5份。本发明利用膨胀石墨在高温下受热可迅速膨胀，膨胀倍数可达到数十倍及上千倍，膨胀后石墨的表观容积可达到250ml以上，在内部形成大量独特的网络状微孔结构,将其与有机树脂如硅树脂进行复合，经过一定温度条件，形成具有阻燃自灭火性能的片材、卷材或不规则异型构件；同时运用高速动态真空混合技术加速体系混合，防止团聚，提高分散效果，使膨胀石墨与树脂充分混合。

Description

一种膨胀石墨阻燃灭火材料及其制备方法
技术领域
本发明属于导热防火材料技术领域，具体地说，涉及一种膨胀石墨阻燃灭火材料及其制备方法。
背景技术
随着电子产品的日益发展，消费电子产品正日益压缩其结构空间。与此同时，随着硬件技术的革新，电子产品的发热问题，成为设计人员和消费者关注的问题，发热问题影响电子产品的寿命及消费者的安全。
阻燃材料的应用，降低了汽车、电子电气、交通运输和航天航空等领域因火灾引起的损失，随着以有机硅功能性材料在电子电器等领域的广泛推广应用，尤其是LED的需求迅速扩大，对使用材料有了更高的要求，既要满足欧盟RoHS(Restriction of HazardousSubstances，关于限制在电子电器设备中使用某些有害成分的指令)环保要求，又要符合REACH指令要求，现有的导热材料及导电材料还无法做到同时具有优良的导热性能及无卤阻燃性能，限制了材料在电子电器设备领域的应用推广。
目前阻燃材料的类别主要分为有机和无机，卤素和非卤。高阻燃材料有机是以溴系、氮系和红磷及化合物为代表的一些阻燃剂，无机主要有三氧化二锑、氢氧化镁、氢氧化铝及硅系等阻燃体系。一般来讲有机阻燃具有很好的亲和力，溴系阻燃剂在有机阻燃体系中占据绝对优势，虽然在环保问题上“非议”多，但一直难以有其他阻燃剂体系取代。
而膨胀石墨在高温下受热可迅速膨胀，膨胀倍数可达到数十倍及上千倍，膨胀后石墨的表观容积可达到250ml以上，在内部形成大量独特的网络状微孔结构，可以作为阻燃剂使用。
针对上述现有技术，结合膨胀石墨的特性设计开发了利用膨胀石墨填充硅树脂、环氧树脂等有机树脂体系，制作具有高导热、高导电或导电导热涂层阻燃防火材料，使其在功能材料及涂料领域具有规模化实际使用的前景。
发明内容
有鉴于此，本发明提供了一种膨胀石墨阻燃灭火材料，其包括以下重量份的组分：
有机树脂5～40份
膨胀石墨粉0.5～30份
导热导电粉体10～80份
偶联剂1～10份
固化剂0.5～5份
助剂0.5～5份。
根据本申请的一实施方式，上述有机树脂为氟碳树脂、氨基树脂、酚醛树脂、丙烯酸树脂、环氧树脂、水溶性树脂及有机硅树脂的一种。
根据本申请的一实施方式，上述膨胀石墨粉包含不同膨胀倍数的膨胀石墨，膨胀倍数为50～400倍。
根据本申请的一实施方式，上述导热导电粉包括氧化铝、氮化硼、氧化镁、石墨烯、纳米碳、碳纳米管、金属镍、镍包石墨、镍包铝、镍包铜等粉体中的一种或几种。
根据本申请的一实施方式，上述助剂包括附着力促进剂、偶联剂、分散剂、流平剂或消泡剂中的一种或多种。
本发明还公开了一种膨胀石墨阻燃灭火材料的制备方法，其特征在于，包括以下步骤：
将偶联剂与导热导电粉体分散混合，偶联剂包覆于导热导电粉体的表面，形成导电填料；
将导电填料与所述有机树脂、固化剂、膨胀石墨及助剂装入高速分散机混合分散，分散1分钟～1个小时，并真空除气，形成导电胶液；及
压延或涂布所述导电胶液，形成片材、卷材或异性构件，并加热烘烤定型，加热温度为120℃～150℃，加热时间为10～30min。
与现有技术相比，本发明可以获得包括以下技术效果：
(1)利用膨胀石墨在高温下受热可迅速膨胀，膨胀倍数可达到数十倍及上千倍，膨胀后石墨的表观容积可达到250ml以上，在内部形成大量独特的网络状微孔结构,将其与有机树脂如硅树脂进行复合，经过一定温度条件，形成具有阻燃自灭火性能的片材、卷材或不规则异型构件；
(2)运用高速动态真空混合技术加速体系混合，防止团聚，提高分散效果，使膨胀石墨与树脂充分混合。
当然，实施本发明的任一产品必不一定需要同时达到以上所述的所有技术效果。
具体实施方式
以下将揭露本申请的多个实施方式，为明确说明起见，许多实务上的细节将在以下叙述中一并说明。然而，应了解到，这些实务上的细节不应用以限制本申请。也就是说，在本申请的部分实施方式中，这些实务上的细节是非必要的。
实施例一
将3份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、0.5份膨胀石墨及2.5份助剂装入高速分散机混合分散，助剂为分散剂和流平剂，分散时间为5分钟,分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液A。将导电胶液A压延或者涂布在基材PET塑料上，于130℃高温加热20min,烘烤交联固化，定型成为片材、卷材或异性构件。
实施例二
将3份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、1份膨胀石墨及2.5份助剂装入高速分散机混合分散，助剂为分散剂和流平剂，分散时间为5分钟，分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液B。将导电胶液B压延或者涂布在基材PET塑料上，于130℃高温加热20min,烘烤交联固化，定型成为片材、卷材或异性构件。
实施例三
将3份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、1.5份膨胀石墨及2.5份助剂装入高速分散机混合分散，助剂为分散剂和流平剂，分散时间为5分钟,分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液C。将导电胶液C压延或者涂布在基材PET塑料上，于130℃高温加热20min,烘烤交联固化，定型成为片材、卷材或异性构件。
实施例四
将1份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、2份膨胀石墨及2.5份助剂装入高速分散机混合分散,助剂为分散剂和流平剂，分散时间为5分钟,分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液D。将导电胶液D压延或者涂布在基材PET塑料上，于130℃高温加热20min,定型成为片材、卷材或异性构件。
实施例五
将1份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、0.5份膨胀石墨及2.5份助剂装入高速分散机混合分散，助剂为分散剂和流平剂，分散时间为5分钟,分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液E。将导电胶液E压延或者涂布在基材PET塑料上，于130℃高温加热20min,烘烤交联固化，定型成为片材、卷材或异性构件。
实施例六
将3份偶联剂和60份导热导电粉体高速分散，对导热导电粉体进行表面处理，偶联剂在热导电粉体的表面均匀包覆，二者混合形成导电填料，从而增强导电填料与后续树脂基体混合时的相容性。再将导电填料与40份有机树脂、2份固化剂、0.5份膨胀石墨及2.5份助剂装入高速分散机混合分散，助剂为分散剂和流平剂，分散时间为5分钟,分散速度为800转/分钟；分散完毕后真空除气，形成导电胶液F。将导电胶液F压延或者涂布在基材PET塑料上，于130℃高温加热20min,烘烤交联固化，定型成为片材、卷材或异性构件。
在相同环境和温度下测试上述四个实施例的制成的导电胶液A、导电胶液B、导电胶液C、导电胶液D、导电胶液E和导电胶液F固化后的产品的阻燃等级和击穿电压，数据如下表一所示。
表一
从表一可以看出六个实施例中的组分的比例的调整所引起的阻燃等级和击穿电压的变化，随膨胀石墨粉比例的增加，所制备材料的阻燃灭火性能越强，最少添加比例不能小于1％，B和C组份添加比例比较合适，绝缘性能随着膨胀石墨粉比例增加而下降。
综上所述，本发明可以获得包括以下技术效果：
(1)利用膨胀石墨在高温下受热可迅速膨胀，膨胀倍数可达到数十倍及上千倍，膨胀后石墨的表观容积可达到250ml以上，在内部形成大量独特的网络状微孔结构,将其与有机树脂如硅树脂进行复合，经过一定温度条件，制作片材、卷材或不规则异型构件，提高体系阻燃性能；
(2)运用高速动态真空混合技术加速体系混合，防止团聚，提高分散效果，使膨胀石墨与树脂充分混合。
还需要说明的是，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商品或者***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商品或者***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商品或者***中还存在另外的相同要素。
上述说明示出并描述了本发明的若干优选实施例，但如前所述，应当理解本发明并非局限于本文所披露的形式，不应看作是对其他实施例的排除，而可用于各种其他组合、修改和环境，并能够在本文所述发明构想范围内，通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围，则都应在本发明所附权利要求的保护范围内。

Claims (6)

1.一种膨胀石墨阻燃灭火材料，其特征在于，包括以下重量份的组分：
有机树脂5～40份
膨胀石墨粉0.5～30份
导热导电粉体10～80份
偶联剂1～10份
固化剂0.5～5份
助剂0.5～5份。
2.根据权利要求1所述的膨胀石墨阻燃灭火材料，其特征在于，所述有机树脂为氟碳树脂、氨基树脂、酚醛树脂、丙烯酸树脂、环氧树脂、水溶性树脂及有机硅树脂的一种。
3.根据权利要求1所述的膨胀石墨阻燃灭火材料，其特征在于，所述膨胀石墨粉包含不同膨胀倍数的膨胀石墨，膨胀倍数为50～400倍。
4.根据权利要求1至3任一所述的膨胀石墨阻燃灭火材料，其特征在于，所述导热导电粉包括氧化铝、氮化硼、氧化镁、石墨烯、纳米碳、碳纳米管、金属镍、镍包石墨、镍包铝、镍包铜等粉体中的一种或几种，优选氧化铝、纳米碳、镍包石墨。
5.根据权利要求4所述的膨胀石墨阻燃灭火材料，其特征在于，所述助剂包括附着力促进剂、偶联剂、分散剂、流平剂或消泡剂中的一种或多种。
6.一种根据权利要求1、2、3或5任一所述的膨胀石墨阻燃灭火材料的制备方法，其特征在于，包括以下步骤：
将所述偶联剂与所述导热导电粉体分散混合，所述偶联剂包覆于所述导热导电粉体表面，形成导电填料；
将所述导电填料与所述有机树脂、固化剂、膨胀石墨及助剂装入高速分散机混合分散，分散1分钟～1个小时，并真空除气，形成导电胶液；及
压延或涂布所述导电胶液，形成片材、卷材或异型构件，并加热烘烤定型，加热温度为120℃～150℃，加热时间为10～30min。
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