CN107746548A - 耐高温树脂基体及其制造方法 - Google Patents

耐高温树脂基体及其制造方法 Download PDF

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CN107746548A
CN107746548A CN201711089015.XA CN201711089015A CN107746548A CN 107746548 A CN107746548 A CN 107746548A CN 201711089015 A CN201711089015 A CN 201711089015A CN 107746548 A CN107746548 A CN 107746548A
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fire resistant
resin matrix
resistant resin
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曾秋云
林凤森
丛庆
李盛林
王大伟
李琳
郭辉
严红超
李刚
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Weihai Guangwei Composites Co Ltd
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Abstract

本发明涉及一种耐高温树脂基体及其制造方法，属于高分子材料领域。原料以质量份数计，含有65‑80质量份的多官能度环氧树脂，8‑15质量份的增韧剂，10‑25质量份的双酚A型环氧树脂，15‑30质量份的固化剂，以及0.1‑8质量份的固化促进剂。该配方设计的耐高温树脂基体不仅具有优异的工艺性，而且用此树脂基体制备的复合材料具有高耐热性，高强度，高冲击性，高抗蚀等优异性能。并且，该树脂的制造方法避免了多官能度环氧树脂在高温下发生爆聚的风险。

Description

耐高温树脂基体及其制造方法
技术领域
本发明涉及高分子材料领域，详细地讲是一种耐高温树脂基体及其制造方法。
背景技术
众所周知，兼具韧性和耐热性的环氧树脂一直是研究的热点。用刚性无机填料，如玻璃微球、氢氧化铝，增韧效果不明显。用橡胶弹性体口进行增韧改性，会在提高韧性的同时大大降低其玻璃化转变温度。采用互穿网络聚合物(IPN)方法增韧，相态结构在影响IPN性能因素中占有主导地位，须控制界面张力、交联密度、聚合方法以及IPN的组分等条件；采用高性能工程塑料，如聚砜、聚醚砜、聚醚酰亚胺，聚酰亚胺等来增韧改性环氧树脂，不仅能提高和改善环氧树脂的韧性，而且也不会牺牲其它高温机械方面的优异性能。
发明内容
为了克服现有技术的不足，本发明提供一种耐高温树脂基体及其制造方法，制备的树脂不仅具有优良的工艺性，而且用此树脂基体制备的复合材料具有高耐热性，高强度，高冲击性，高抗蚀等优异性能。并且，该树脂的制造方法可以避免多官能度环氧树脂在高温下发生爆聚的风险。
本发明解决其技术问题所采用的技术方案是：一种耐高温树脂基体及其制造方法，其特征在于，原料以质量份数计，含有65-80质量份的多官能度环氧树脂，8-15质量份的增韧剂，10-25质量份的双酚A型环氧树脂，15-30质量份的固化剂，以及0.1-8质量份的固化促进剂。
所述的多官能度环氧树脂包括四缩水甘油基二甲苯二胺、四缩水甘油基二氨基二苯基甲烷、间苯二甲胺四缩水甘油胺、4,5环氧环氧环己烷-1,2二甲酸二缩水甘油酯、三缩水甘油基-p-氨基苯酚中的一种或多种。
所述的增韧剂为粒径≤50μm的聚醚砜，聚芳醚酮，聚醚醚酮，聚砜，聚苯醚等热塑性树脂或甲基丙烯酸甲酯-丙烯酸丁酯-甲基丙烯酸甲酯三嵌段共聚物中的一种或多种。
所述的双酚A型环氧树脂为液态，为NPEL127、NPEL127E、NPEL128、NPEL128E、NPEL128R、NPEL128W、DER300、DER331、NPEL128S中的一种或几种。
所述的固化剂为4,4′-二氨基二苯砜，4,4′-二氨基二苯甲烷，间苯二胺，间苯二甲胺中的一种或几种。
所述的固化促进剂为改性咪唑、有机磷化合物、三氟化硼络合物中的一种或多种。
一种制备前述耐高温树脂基体的方法，其特征在于包括下列步骤：
将配方量的增韧剂分批次加入到140-150℃配方量的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份；
将2/5倍配方量的多官能度的环氧树脂加入到配方量的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份；
将配方量的固化剂和固化促进剂加入到3/5倍配方量的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份；
将配方量的C组份加入到配方量的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
本发明的有益效果是，该配方设计的耐高温树脂基体不仅具有优异的工艺性，而且用此树脂基体制备的复合材料具有高耐热性，高强度，高冲击性，高抗蚀等优异性能。并且，该树脂的制造方法避免了多官能度环氧树脂在高温下发生爆聚的风险。
具体实施方式
下面结合实施例对本发明进一步说明。
实施案例1：
设备：本发明所需要的设备有：搅拌器，配有加热，温控器以及抽真空系统的高温反应釜和中温反应釜，真空烘箱，真空泵，鼓风干燥烘箱。
将15质量份的增韧剂分批次加入到140-150℃的10质量份的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份。
将32质量份的多官能度的环氧树脂加入到25质量份的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份。
将20质量份的固化剂和8质量份的固化促进剂加入到48质量份的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份。
将76质量份的C组份加入到57质量份的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
将上述制备好的耐高温树脂基体在70℃-80℃真空烘箱中，至树脂全部融化，打开真空泵，进行脱泡，脱泡时间为15-20min。然后将脱泡后的树脂倒入预热的模具中，然后放入鼓风干燥烘箱中进行升温固化，其工艺为：120℃/2h+150℃/2h+180℃/2h。然后，自然冷却，脱模，再根据相应的测试标准测试树脂的力学性能及耐热性。玻璃化转变温度为202.48℃，拉伸强度35.27MPa，拉伸弹性模量2.34GPa，断裂伸长率2.01%，弯曲强度48.61MPa，弯曲模量2.13GPa。
实施案例2：
设备：同实施方案1
将13质量份的增韧剂分批次加入到140-150℃的15质量份的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份。
将30质量份的多官能度的环氧树脂加入到28质量份的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份。
将20质量份的固化剂和6质量份的固化促进剂加入到45质量份的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份。
将71质量份的C组份加入到58质量份的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
同实施案例1制备树脂浇筑体，经测试，玻璃化转变温度为20315℃，拉伸强度43.54MPa，拉伸弹性模量2.68GPa，断裂伸长率2.61%，弯曲强度57.14MPa，弯曲模量2.85GPa。
实施案例3：
设备：同实施方案1
将11质量份的增韧剂分批次加入到140-150℃的20质量份的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份。
将28质量份的多官能度的环氧树脂加入到31质量份的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份。
将25质量份的固化剂和5质量份的固化促进剂加入到42质量份的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份。
将72质量份的C组份加入到59质量份的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
同实施案例1制备树脂浇筑体，经测试，玻璃化转变温度为207.28℃，拉伸强度62.34MPa，拉伸弹性模量3.31GPa，断裂伸长率3.15%，弯曲强度89.57MPa，弯曲模量3.34GPa。
实施案例4：
设备：同实施方案1
将9质量份的增韧剂分批次加入到140-150℃的25质量份的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份。
将26质量份的多官能度的环氧树脂加入到34质量份的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份。
将25质量份的固化剂和5质量份的固化促进剂加入到39质量份的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份。
将69质量份的C组份加入到60质量份的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
同实施案例1制备树脂浇筑体，经测试，玻璃化转变温度为196.21℃，拉伸强度50.27MPa，拉伸弹性模量2.75GPa，断裂伸长率2.63%，弯曲强度67.81MPa，弯曲模量2.84GPa。

Claims (7)

1.一种耐高温树脂基体，其特征在于，原料以质量份数计，含有65-80质量份的多官能度环氧树脂，8-15质量份的增韧剂，10-25质量份的双酚A型环氧树脂，15-30质量份的固化剂，以及0.1-8质量份的固化促进剂。
2.根据权利要求1所述耐高温树脂基体，其特征在于所述的多官能度环氧树脂包括四缩水甘油基二甲苯二胺、四缩水甘油基二氨基二苯基甲烷、间苯二甲胺四缩水甘油胺、4,5环氧环氧环己烷-1,2二甲酸二缩水甘油酯、三缩水甘油基-p-氨基苯酚中的一种或多种。
3.根据权利要求1所述耐高温树脂基体，其特征在于所述的增韧剂为粒径≤50μm的聚醚砜，聚芳醚酮，聚醚醚酮，聚砜，聚苯醚等热塑性树脂或甲基丙烯酸甲酯-丙烯酸丁酯-甲基丙烯酸甲酯三嵌段共聚物中的一种或多种。
4.根据权利要求1所述耐高温树脂基体，其特征在于所述的双酚A型环氧树脂为液态，为NPEL127、NPEL127E、NPEL128、NPEL128E、NPEL128R、NPEL128W、DER300、DER331、NPEL128S中的一种或几种。
5.根据权利要求1所述耐高温树脂基体，其特征在于所述的固化剂为4,4′-二氨基二苯砜，4,4′-二氨基二苯甲烷，间苯二胺，间苯二甲胺中的一种或几种。
6.根据权利要求1所述耐高温树脂基体，其特征在于所述的固化促进剂为改性咪唑、有机磷化合物、三氟化硼络合物中的一种或多种。
7.一种制备权利要求1所述耐高温树脂基体的方法，其特征在于，包括下列步骤：
将配方量的增韧剂分批次加入到140-150℃配方量的双酚A环氧树脂中，搅拌2-2.5h，至增韧剂全部熔融，混合溶液均匀一致，此混合溶液称为A组份；
将2/5倍配方量的多官能度的环氧树脂加入到配方量的A组份中，溶液温度在100-110℃范围内，搅拌时间10-15min，至混合溶液均匀一致，此时的溶液称为B组份；
将配方量的固化剂和固化促进剂加入到3/5倍配方量的多官能度的环氧树脂中，进行搅拌，混合物浓度一直保持在≤70℃范围内，搅拌时间20-25min，搅拌完成后，进行三辊研磨，研磨两到三次，此时的混合物称为C组份；
将配方量的C组份加入到配方量的B组份中，温度设置在60-70范围，搅拌时间15-20min，即得到耐高温树脂基体。
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