化学研究
化學研究
화학연구
CHEMICAL RESEARCHES
2013年
6期
564-568
,共5页
余丽丽%任艳蓉%丁涛%徐元清%徐浩%胡永佳%房晓敏%崔志萍
餘麗麗%任豔蓉%丁濤%徐元清%徐浩%鬍永佳%房曉敏%崔誌萍
여려려%임염용%정도%서원청%서호%호영가%방효민%최지평
六氯环三磷腈%苯并噁嗪树脂%合成%结构%热稳定性
六氯環三燐腈%苯併噁嗪樹脂%閤成%結構%熱穩定性
륙록배삼린정%분병오진수지%합성%결구%열은정성
hexachlorocyclotriphosphazene%benzoxazine resin%synthesis%structure%thermal stability
以双螺环取代三聚磷腈基双苯甲酰氯和4-氨基(N-苯基)苯并噁嗪单体为原料合成了一种含双螺环取代三聚磷腈结构单元的苯并噁嗪树脂单体(HCP-5);采用傅立叶变换红外光谱仪(FT-IR)和核磁共振谱仪(1 H NMR ,13C NMR ,31P NMR)表征了苯并噁嗪树脂单体的结构,基于 FT-IR和示差扫描量热法研究了其固化行为,并利用热重分析和示差热重分析研究了HCP-5树脂单体、均聚物及其与双酚A型苯并噁嗪树脂(Bz)共聚物的热稳定性。结果表明,HCP-5均聚物具有很好的热稳定性和成炭性,其在317℃下的热失重为5%,在800℃下的残炭率为50%,可用于普通苯并噁嗪树脂改性。此外,H C P-5/Bz (1∶1;质量分数)共聚物在332℃下的热失重为5%,在800℃下的残炭率为48%。
以雙螺環取代三聚燐腈基雙苯甲酰氯和4-氨基(N-苯基)苯併噁嗪單體為原料閤成瞭一種含雙螺環取代三聚燐腈結構單元的苯併噁嗪樹脂單體(HCP-5);採用傅立葉變換紅外光譜儀(FT-IR)和覈磁共振譜儀(1 H NMR ,13C NMR ,31P NMR)錶徵瞭苯併噁嗪樹脂單體的結構,基于 FT-IR和示差掃描量熱法研究瞭其固化行為,併利用熱重分析和示差熱重分析研究瞭HCP-5樹脂單體、均聚物及其與雙酚A型苯併噁嗪樹脂(Bz)共聚物的熱穩定性。結果錶明,HCP-5均聚物具有很好的熱穩定性和成炭性,其在317℃下的熱失重為5%,在800℃下的殘炭率為50%,可用于普通苯併噁嗪樹脂改性。此外,H C P-5/Bz (1∶1;質量分數)共聚物在332℃下的熱失重為5%,在800℃下的殘炭率為48%。
이쌍라배취대삼취린정기쌍분갑선록화4-안기(N-분기)분병오진단체위원료합성료일충함쌍라배취대삼취린정결구단원적분병오진수지단체(HCP-5);채용부립협변환홍외광보의(FT-IR)화핵자공진보의(1 H NMR ,13C NMR ,31P NMR)표정료분병오진수지단체적결구,기우 FT-IR화시차소묘량열법연구료기고화행위,병이용열중분석화시차열중분석연구료HCP-5수지단체、균취물급기여쌍분A형분병오진수지(Bz)공취물적열은정성。결과표명,HCP-5균취물구유흔호적열은정성화성탄성,기재317℃하적열실중위5%,재800℃하적잔탄솔위50%,가용우보통분병오진수지개성。차외,H C P-5/Bz (1∶1;질량분수)공취물재332℃하적열실중위5%,재800℃하적잔탄솔위48%。
A benzoxazine resin monomer (coded as HCP-5) containing bis-spiro-substituted cy-clotriphosphazene structural unit was synthesized with hexachlorocyclotriphosphazene-2 ,2′-bi-phenol formyl chloride and 4-amino-N-phenyl benzoxazine as the starting materials .The struc-ture of as-synthesized HCP-5 resin monomer was confirmed by Fourier transform infrared spec-trometry (FT-IR) and nuclear magnetic resonance spectroscopy (1 H NM R ,13 C NM R and 31 P NMR) .The curing behavior of HCP-5 resin monomer was investigated based on FT-IR analy-sis and differential scanning calorimetric analysis ,w hile the thermal stability of HCP-5 resin monomer and homopolymer as well as the copolymer of HCP-5 monomer with bisphenol-based benzoxazine (Bz) was evaluated by thermogravimetric analysis and differential thermogravimet-ric analysis .Results show that the homopolymer of HCP-5 has excellent thermal stability and char-formation ability .Namely ,it loses 5% of weight at 317 ℃ under nitrogen atmosphere and has a char yield of 50% at 800 ℃ , showing potential for the modification of conventional benzoxazine resin .Besides , the copolymer of HCP-5 monomer with Bz , HCP-5/Bz (1 ∶ 1 ;mass ratio) ,loses 5% of weight at 332 ℃ and yields 48% of char at 800 ℃ .