CN108794981A - 阻燃型环氧树脂及其制备方法 - Google Patents

阻燃型环氧树脂及其制备方法 Download PDF

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CN108794981A
CN108794981A CN201810327131.9A CN201810327131A CN108794981A CN 108794981 A CN108794981 A CN 108794981A CN 201810327131 A CN201810327131 A CN 201810327131A CN 108794981 A CN108794981 A CN 108794981A
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epoxy resin
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薛兆能
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Anhui Wandong Resin Technology Co Ltd
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/68Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
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    • 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
    • C08K2201/011Nanostructured additives
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Epoxy Resins (AREA)

Abstract

本发明公开一种阻燃型环氧树脂及其制备方法,以质量份数计,包括以下组分:二酚基丙烷型环氧树脂60~80份,邻苯二甲腈树脂2~10份,纳米无机填料200~240份,固化剂5~10份,促进剂0.5~2份,阻燃剂1~10份。本发明制得的环氧树脂抗湿性更强,粘度更低,可操作性更强,出现明火的时间显著提高,且弯曲强度及拉伸模量均有显著提升。

Description

阻燃型环氧树脂及其制备方法
技术领域
本发明涉及电子元器件领域,具体涉及一种阻燃型环氧树脂及其制备方法。
背景技术
环氧树脂是指分子中含有两个以上环氧基团的一类聚合物的总称。它是环氧氯丙烷与双酚A或多元醇的缩聚产物。由于环氧基的化学活性,可用多种含有活泼氢的化合物使其开环,固化交联生成网状结构,因此它是一种热固性树脂。环氧树脂以其绝缘性能高、结构强度大和密封性能好、成本低廉的优点被广泛应用于电子元器件领域。
由于普通环氧树脂材料制成的电子器件在高温时会分解发烟并伴有明火的缺点,限制了环氧树脂的应用,存在很大的安全隐患。
发明内容
本发明提供一种阻燃型环氧树脂及其制备方法,阻燃效果好、操作简单。
为了实现上述目的,本发明采用以下技术方案:
一种阻燃型环氧树脂,以质量份数计,包括以下组分:二酚基丙烷型环氧树脂60~80份,邻苯二甲腈树脂2~10份,纳米无机填料200~240份,固化剂5~10份,促进剂0.5~2份,阻燃剂1~10份。
进一步的,所述的纳米无机填料为纳米二氧化硅。
进一步的,所述的固化剂为异佛尔酮二胺,促进剂为水杨酸和苯甲醇的混合物。水杨酸与苯甲醇的比例为1:7时固化效果最佳,通过水杨酸和苯甲醇的协同作用,即使在室温条件下,也可实现均匀快速的固化。
进一步的,所述的阻燃剂为季戊四醇磷酸酯的三聚氰胺盐。
一种根据权利要求1所述的阻燃型环氧树脂的制备方法,其特征在于:包括以下步骤:
1)将二酚基丙烷型环氧树脂60~80份,邻苯二甲腈树脂2~10份,纳米无机填料200~240份,在反应釜中搅拌混合,在80~120℃温度下反应4-8H;
2)将固化剂5~10份,促进剂0.5~2份,阻燃剂1~10份,加入步骤1)反应后的溶液中,室温下混合均匀,得到阻燃型环氧树脂。
进一步的,步骤2)中反应的时间为6-8H。
进一步的,所述的环氧树脂的环氧值≥0.8。
与现有技术相比,本发明的的有益效果为:本发明提供的阻燃型环氧树脂,各组分之间相互配伍产生协同作用,本发明采用纳米二氧化硅,通过与环氧树脂的协同作用,使制成的环氧树脂强度硬度提高,抗老化性增加;
本发明采用的固定剂为异佛尔酮二胺,促进剂为水杨酸和苯甲醇的混合物。通过水杨酸和苯甲醇的协同作用,即使在室温条件下,也可实现均匀快速的固化
本发明制得的阻燃型环氧树脂的阻燃型耐热性满足400~500℃无明火,可被用于电阻元件的封装,且本发明制得的阻燃型环氧树脂有良好的强度硬度、抗老化性及耐湿性能,特别适合用于制作浴室电器元件。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1
以质量份数计,将二酚基丙烷型环氧树脂60份,环氧树脂的环氧值0.8,邻苯二甲腈树脂2份,纳米二氧化硅200份,在反应釜中搅拌混合,在80℃温度下反应4H;将异佛尔酮二胺5份,水杨酸和苯甲醇的混合物0.5份,季戊四醇磷酸酯的三聚氰胺盐1份,加入反应后的溶液中,室温下混合均匀,反应的时间为6H,得到阻燃型环氧树脂。详细数据信息见表1。
实施例2
以质量份数计,将二酚基丙烷型环氧树脂80份,环氧树脂的环氧值0.9,邻苯二甲腈树脂10份,纳米二氧化硅240份,在反应釜中搅拌混合,在120℃温度下反应8H;将异佛尔酮二胺10份,水杨酸和苯甲醇的混合物2份,季戊四醇磷酸酯的三聚氰胺盐10份,加入反应后的溶液中,室温下混合均匀,反应的时间为8H,得到阻燃型环氧树脂。详细数据信息见表1。
实施例3
以质量份数计,将二酚基丙烷型环氧树脂70份,环氧树脂的环氧值0.8,邻苯二甲腈树脂6份,纳米二氧化硅220份,在反应釜中搅拌混合,在100℃温度下反应6H;将异佛尔酮二胺7份,水杨酸和苯甲醇的混合物1份,季戊四醇磷酸酯的三聚氰胺盐5份,加入反应后的溶液中,室温下混合均匀,反应的时间为7H,得到阻燃型环氧树脂。详细数据信息见表1。
对照例1
以质量份数计,将二酚基丙烷型环氧树脂60份,环氧树脂的环氧值0.6,二氧化硅200份,在反应釜中搅拌混合,在80℃温度下反应4H,将异佛尔酮二胺5份,季戊四醇磷酸酯的三聚氰胺盐1份,加入反应后的溶液中,室温下混合均匀,反应的时间为6H,得到阻燃型环氧树脂。详细数据信息见表1。
表1
*水混溶性指:体积水:1体积固化剂
由表1可知,通过加入固化剂异佛尔酮二胺与水的混溶性下降,抗湿性更强,加入水杨酸和苯甲醇作为促进剂,粘度更低,可操作性更强,出现明火的时间显著提高,且弯曲强度及拉伸模量均有显著提升。
以上显示和描述了本发明的基本原理、主要特征和本发明的特点。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的范围内。本发明要求保护的范围由所附的权利要求书及其等效物界定。

Claims (7)

1.一种阻燃型环氧树脂,其特征在于:以质量份数计,包括以下组分:二酚基丙烷型环氧树脂60~80份,邻苯二甲腈树脂2~10份,纳米无机填料200~240份,固化剂5~10份,促进剂0.5~2份,阻燃剂1~10份。
2.根据权利要求1所述的阻燃型环氧树脂,其特征在于:所述的纳米无机填料为纳米二氧化硅。
3.根据权利要求1所述的阻燃型环氧树脂,其特征在于:所述的固化剂为异佛尔酮二胺,促进剂为水杨酸和苯甲醇的混合物。
4.根据权利要求1所述的阻燃型环氧树脂,其特征在于:所述的阻燃剂为季戊四醇磷酸酯的三聚氰胺盐。
5.一种根据权利要求1所述的阻燃型环氧树脂的制备方法,其特征在于:包括以下步骤:
1)将二酚基丙烷型环氧树脂60~80份,邻苯二甲腈树脂2~10份,纳米无机填料200~240份,在反应釜中搅拌混合,在80~120℃温度下反应4-8H;
2)将固化剂5~10份,促进剂0.5~2份,阻燃剂1~10份,加入步骤1)反应后的溶液中,室温下混合均匀,得到阻燃型环氧树脂。
6.根据权利要求5所述的阻燃型环氧树脂的制备方法,其特征在于:步骤2)中反应的时间为6-8H。
7.根据权利要求5所述的阻燃型环氧树脂的制备方法,其特征在于:所述的环氧树脂的环氧值≥0.8。
CN201810327131.9A 2018-04-12 2018-04-12 阻燃型环氧树脂及其制备方法 Pending CN108794981A (zh)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113201302A (zh) * 2021-05-06 2021-08-03 黑龙江省科学院石油化学研究院 一种双氨基双邻苯二甲腈改性环氧树脂胶粘剂及其制备方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5939508A (en) * 1995-09-01 1999-08-17 The United States Of America As Represented By The Secretary Of The Navy High temperature epoxy-phthalonitrile blends
CN105229095A (zh) * 2012-12-14 2016-01-06 蓝立方知识产权有限责任公司 高含固量环氧树脂涂料
CN107663360A (zh) * 2016-07-28 2018-02-06 航天特种材料及工艺技术研究所 一种耐高温阻燃环氧树脂及制备方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5939508A (en) * 1995-09-01 1999-08-17 The United States Of America As Represented By The Secretary Of The Navy High temperature epoxy-phthalonitrile blends
CN105229095A (zh) * 2012-12-14 2016-01-06 蓝立方知识产权有限责任公司 高含固量环氧树脂涂料
CN107663360A (zh) * 2016-07-28 2018-02-06 航天特种材料及工艺技术研究所 一种耐高温阻燃环氧树脂及制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113201302A (zh) * 2021-05-06 2021-08-03 黑龙江省科学院石油化学研究院 一种双氨基双邻苯二甲腈改性环氧树脂胶粘剂及其制备方法
CN113201302B (zh) * 2021-05-06 2023-03-03 黑龙江省科学院石油化学研究院 一种双氨基双邻苯二甲腈改性环氧树脂胶粘剂及其制备方法

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Application publication date: 20181113