首先以双环戊二烯和呋喃甲胺为原料,通过Diels-Alder反应合成了中间单体双环戊烯-呋喃甲胺(DCPD-F),然后用DCPD-F与双酚A、甲醛为原料进行曼尼希反应合成了带有桥环结构的苯并噁嗪(DCPD-F-BOZ),经过高温固化形成热固性树脂poly(DCPD-F-BOZ)。采用红外光谱、核磁共振仪等手段表征DCPD-F和DCPD-F-BOZ的化学结构;采用差示量热分析DCPD-F-BOZ的固化特性;采用热重分析了poly(DCPD-F-BOZ)的热稳定性后测试其介电常数。结果表明:DCPD-F-BOZ在223℃和258℃出现了两个固化峰;在N2条件下,poly(DCPD-F-BOZ)的热分解温度为360℃,失重5%的温度为382℃,在800℃的残炭率为53%。室温下介电常数为2.76(1GHz)。
The intermediate monomer dicyclopentene-furanmethylamine (DCPD-F) was firstly synthesized by Diels-Alder reaction using dicyclopentadiene and furanmethylamine as raw materials.And then the synthesized(DCPD-F) and bisphenol A and formaldehyde were used as raw materials through Mannich reaction to synthesize a benzoxazine(DCPD-F-BOZ) with bridged rings structure,which was cured at high temperature to form a thermosetting resin.The chemical structure of DCPD-F and DCPD-F-BOZ was characterized by FT-IR and NMR.The curing behavior of DCPD-F-BOZ was characterized by DSC,which two peaks at about 223℃ and 258℃ appeared during its curing,respectively.The themal stability of poly(DCPD-F-BOZ) was analyzed by TGA,with the dielectric constant being tested.The results showed that poly(DCPD-F-BOZ) had excellent thermal stability under the condition of nitrogen,which began to decompose at 360℃ with 5% mass loss temperature of 382℃.The char yield rate at 800℃ was 53% and the dielectric constant at room temperature was 2.96(1GHz).
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基金资助
国家自然科学基金(51273054)
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