CN105924902B - 一种可热膨胀的固体环氧树脂微孔发泡材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种可热膨胀的固体环氧树脂微孔发泡材料及其制备方法,包含以下组份且各组份按照重量计算为:固态环氧树脂40~80份,固化剂30‑50份,无机粒子3~10份,化学发泡剂0.05~5份,增韧剂1~15份,增强纤维0~10份;制备时将前述组合物置于热压机中,在10~25MPa压力下压实;放入预留有发泡空间的发泡模具中在90~160℃发泡成型2~4h;然后升高温度至180~200℃后处理3h,冷却后脱模即可。本发明的发泡材料具有很好的物理机械性能,易于加工,方便储存运输,膨胀后泡孔结构均匀规则,有效的解决了现有方法制备的固态可热膨胀材料泡孔尺寸大,难以成型加工和不便储存的不足。
Description
技术领域
本发明涉及一种可热膨胀的固体环氧树脂微孔发泡材料及其制备方法,属于环氧树脂微孔发泡材料技术开发及应用领域。
背景技术
环氧发泡材料具有较好的热稳定性、力学性能、绝缘性能、隔热性能以及轻质等优点,已经广泛应用在汽车、电子灌封、飞机制件、船体外壳等领域。环氧发泡材料的制备方法主要有物理发泡法、化学发泡法和中空微球固化成型法。上述方法制备的环氧树脂泡沫材料泡孔尺寸较大、泡孔数量较少,通常达不到微孔材料的要求。
可热膨胀材料可以用于汽车工业和其他若干工业中。其可以作为隔音保温材料,也可以作为结构增强材料。通常的热膨胀材料是由未固化树脂和发泡剂的混合物组成,其在高温下活化发泡而实现热膨胀,这种热膨胀材料存在以下不足:处于未固化状态的可热膨胀材料由于强度低且脆而难以加工;无法长久储存;热膨胀过程中,由于树脂固化放热而使得泡孔结构难以调控,容易形成不规则和不均匀的泡孔,且泡孔尺寸较大。因此,开发一种便于成型加工且热活化过程易于控制的可热膨胀微孔发泡材料具有重要的实用价值。
发明内容
本发明要解决的技术问题是:提供一种可热膨胀的固体环氧树脂微孔发泡材料及其制备方法,以克服现有方法制备的固态可热膨胀材料泡孔尺寸大,难以成型加工和不便储存的不足。
本发明的技术方案:一种可热膨胀的固体环氧树脂微孔发泡材料,包含以下组份且各组份按照重量计算为:固态环氧树脂40~80份,固化剂30~50份,无机粒子3~10份,化学发泡剂0.05~5份,增韧剂1~15份,增强纤维0~10份。
所述固态环氧树脂在室温下呈固态粉末,其含有双酚A型固态环氧树脂,三聚氰胺环氧树脂、脂肪族固态环氧树脂、酚醛型环氧树脂中的任一种或几种。
所述无机粒子为纳米二氧化硅、纳米蒙脱土、纳米碳酸钙、氧化锌中任一种或几种。
所述增韧剂为纳米或微米橡胶粒子。
所述化学发泡剂为碳酸氢钠、4,4-氧代双苯磺酰肼、偶氮二甲酰胺、N,N’-二亚硝基五次甲基四胺中的任一种。
所述增强纤维为玻纤、碳纤、木质纤维素中的任一种。
所述固化剂为固态羧酸酐或对苯二胺。
制备权利要求前述发泡材料的方法,其制备过程为:将由所述固态环氧树脂、固化剂、无机粒子、化学发泡剂、增韧剂和增强纤维构成的组合物置于热压机中,在10~25MPa压力下压实;放入预留有发泡空间的发泡模具中在90~160℃发泡成型2~4h;然后升高温度至180~200℃后处理3h,冷却后脱模即可得到可热膨胀的固体微孔发泡材料。
经发明人测试,本发明发泡材料的玻璃化转变温度为90~150℃;同时本发明发泡材料在70~150℃加热,会再次膨胀,膨胀后的泡孔尺寸仍然小于100μm,膨胀倍率0.25~10倍。
本发明的工作原理:本发明固态环氧树脂粉末组合物具有合适的黏弹性,能够制备出泡孔均匀的微孔发泡材料;在受限的空间中发泡,使发泡剂分解产生的气体压缩在微孔中,从而制备出可热膨胀的固体微孔发泡材料,当温度升高到固体微孔发泡材料的玻璃化转变温度附近时,压缩气体发生膨胀而使材料发生热膨胀。
与现有技术相比,本发明的可热膨胀发泡材料是一种固体微孔发泡材料,具有很好的物理机械性能,易于加工,方便储存运输;由于热活化过程是物理作用而使得膨胀过程平稳易于控制,膨胀后泡孔结构均匀规则。
附图说明
图1为可热膨胀的固体环氧微孔发泡材料热膨胀前的电镜照片;
图2为可热膨胀的固体环氧微孔发泡材料热膨胀后的电镜照片;
图3为不同密度下的可热膨胀的固体环氧微孔发泡的泡孔直径及可热膨胀倍率图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合附图对本发明作进一步地详细描述。
实施例1:
取固态粉末环氧组合物(固态双酚A环氧树脂40份,三聚氰胺环氧树脂20份,酸酐固化剂40份,纳米蒙脱土10份,纳米羧基丁腈胶10份,N,N’-二亚硝基五次甲基四胺0.6份)35g,在15MPa下压实,放入发泡空间为25%的模具中在110℃下发泡,经过4h后,提升烘箱温度至180℃,保温3h后自然冷却至室温脱模得到可热膨胀的固体微孔发泡材料;将该可热膨胀的固体材料放入90度烘箱中,即可自行膨胀。设定模具有不同的发泡空间可以制备不同密度的可热膨胀的固体微孔发泡材料,也可以调控材料的热膨胀倍率。
实验结果:如图1~图2所示,可热膨胀的固体微发泡材料热膨胀后,泡孔平均直径由33μm增大到37μm,表观密度由0.9g/cm3降低到0.4g/cm3。
如图3所示,随着模具预留发泡空间的增大,发泡材料的表观密度不断降低,泡孔尺寸不断增大,可热膨胀的倍率就会降低。
实施例2:
取固态粉末环氧组合物(固态双酚A环氧树脂40份,固态酚醛环氧树脂20份,酸酐固化剂40份,纳米碳酸钙7份,微米丁腈胶8份,碳纤维5份,偶氮二甲酰胺1.2份)35g,在15MPa下压实,放入发泡空间为10%的模具中在150℃下发泡,经过1h后,提升烘箱温度至180℃,保温3h后自然冷却至室温脱模得到可热膨胀的固体微孔发泡材料;将该可热膨胀的固体材料放入110度烘箱中,即可自行膨胀。
经测试,本实施例制备的微孔发泡材料膨胀前的泡孔直径和表观密度分别为30μm和1.1g/cm3,膨胀后材料的泡孔直径和表观密度分别为48μm和0.3g/cm3。
实施例3:
取固态粉末环氧组合物(固态双酚A环氧树脂50份,固态脂肪族环氧树脂10份,对苯二胺40份,氧化锌3份,纳米羧基丁腈胶10份,短玻纤7份,碳酸氢钠2.4份)35g,在15MPa下压实,放入发泡空间为10%的模具中在150℃下发泡,经过1h后,提升烘箱温度至180℃,保温3h后自然冷却至室温脱模得到可热膨胀的固体微孔发泡材料;将该可热膨胀的固体材料放入90度烘箱中,即可自行膨胀。
经测试,本实施例制备的微孔发泡材料膨胀前的泡孔直径和表观密度分别为30μm和1.1g/cm3,膨胀后材料的泡孔直径和表观密度分别为82μm和0.16g/cm3。
实施例4:
取固态粉末环氧组合物(脂肪族固态环氧树脂40份,对苯二胺30份,纳米羧基丁腈胶1份,木质纤维素10份,4,4-氧代双苯磺酰肼0.05份,纳米二氧化硅10份)35g,在15MPa下压实,放入发泡空间为10%的模具中在150℃下发泡,经过1h后,提升烘箱温度至180℃,保温3h后自然冷却至室温脱模得到可热膨胀的固体微孔发泡材料;将该可热膨胀的固体材料放入90度烘箱中,即可自行膨胀。
实施例5:
取固态粉末环氧组合物(脂肪族固态环氧树脂80份,固态羧酸酐50份,微米羧基丁腈胶15份,木质纤维素10份,4,4-氧代双苯磺酰肼5份,氧化锌3份)35g,在15MPa下压实,放入发泡空间为10%的模具中在150℃下发泡,经过1h后,提升烘箱温度至180℃,保温3h后自然冷却至室温脱模得到可热膨胀的固体微孔发泡材料;将该可热膨胀的固体材料放入90度烘箱中,即可自行膨胀。
Claims (7)
1.一种可热膨胀的固体环氧树脂微孔发泡材料的制备方法,其特征在于:发泡材料包含以下组份且各组份按照重量计算为:固态环氧树脂40~80份,固化剂30~50份,无机粒子3~10份,化学发泡剂0.05~5份,增韧剂1~15份,增强纤维0~10份,其制备过程为:将由所述固态环氧树脂、固化剂、无机粒子、化学发泡剂、增韧剂和增强纤维构成的组合物置于热压机中,在10~25MPa压力下压实;放入预留有发泡空间的发泡模具中在90~160℃发泡成型2~4h;然后升高温度至180~200℃后处理3h,冷却后脱模即可得到可热膨胀的固体微孔发泡材料。
2.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述固态环氧树脂在室温下呈固态粉末,其含有双酚A型固态环氧树脂,三聚氰胺环氧树脂、脂肪族固态环氧树脂、酚醛型环氧树脂中的任一种或几种。
3.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述无机粒子为纳米二氧化硅、纳米蒙脱土、纳米碳酸钙、氧化锌中任一种或几种。
4.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述增韧剂为纳米或微米橡胶粒子。
5.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述化学发泡剂为碳酸氢钠、4,4-氧代双苯磺酰肼、偶氮二甲酰胺、N,N’-二亚硝基五次甲基四胺中的任一种。
6.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述增强纤维为玻纤、碳纤、木质纤维素中的任一种。
7.根据权利要求1所述的发泡材料的制备方法,其特征在于:所述固化剂为固态羧酸酐或对苯二胺。
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