低介电性双环戊二烯型苯并口恶嗪的合成及性能

Preparation and Properties of Low Dielectric Dicyclopentadiene Benzoxazines

以双环戊二烯、苯酚为原料通过傅克烷基化反应合成双环戊二烯型酚醛单体(DCPDNO),再用所得的DCPDNO与多聚甲醛、苯胺反应合成双环戊二烯型苯并口恶嗪(DCPD-BOZ)。将所得DCPD-BOZ进行高温固化,DCPD-BOZ与环氧树脂E-51进行熔融共混后经过高温固化。采用傅里叶变换红外光谱、核磁共振(~1H-NMR、^(13)C-NMR)等分析了合成产物的化学结构,证明了产物为目标产物;采用差示扫描量热分析对DCPD-BOZ和DCPD-BOZ/E-51共混物的固化特性进行研究;采用热重分析表征了双环戊二烯型聚苯并口恶嗪poly(DCPD-BOZ)和DCPD-BOZ/E-51共混固化物的热稳定性;测试其介电性。结果表明,DCPD-BOZ在207℃出现了固化峰;在N_2的条件下,poly(DCPD-BOZ)失重5%时温度为301℃,在390℃时热分解速率最快,在800℃的残炭率为35%。在室温下介电常数为2.96,介电损耗为0.019。DCPD-BOZ/E-51共混物在240℃产生热效应;在N_2的条件下,DCPD-BOZ/E-51共混物固化物失重5%时温度为357℃,比poly(DCPD-BOZ)提高了56℃。

Dicyclopentadiene-based phenolic monomer(DCPDNO) was synthesized by Friedel-Crafts reaction using dicyclopentadiene and phenol as raw material. The resulting DCPDNO was reacted with paraformaldehyde and aniline to synthesize dicyclopentadiene-based benzoxazine(DCPD-BOZ). The obtained DCPD-BOZ was mixed with epoxy resin,and then cured at high temperature. The chemical structure of the synthesized product was analyzed by FT-IR, 1H-NMR, 13C-NMR and the like, and the product was proved to be the target product. The curing properties of DCPD-BOZ and DCPD-BOZ/E-51 blends were studied by DSC. the thermal stability of dicyclopentadiene-based benzoxazine poly(DCPD-BOZ) and cured DCPD-BOZ/E-51 blends was studied by TGA,with testing its dielectric property. The results show that DCPD-BOZ has a curing peak at 207 ℃. Under N2 condition, poly(DCPD-BOZ) has the 5% mass loss temperature of 305 ℃, and has the fastest thermal decomposition rate at 390 ℃. The residual carbon rate at 800 ℃ is 35%. Its dielectric constant of room temperature is 2.96,and dissipation factor is 0.019.The DCPD-BOZ/E-51 blends show a reaction peak at 240 ℃ and the DCPD-BOZ/E-51 blends have a mass loss temperature of 357 ℃ under 5%, increased by 56 ℃.