化工学报
化工學報
화공학보
JOURNAL OF CHEMICAL INDUSY AND ENGINEERING (CHINA)
2014年
9期
3694-3700
,共7页
刘建华%史铁钧%徐国梅%王权%王启东
劉建華%史鐵鈞%徐國梅%王權%王啟東
류건화%사철균%서국매%왕권%왕계동
合成%聚合%热稳定性%核磁共振%双酚A-双苯并嗪%含DOPO的双酚A-单苯并嗪
閤成%聚閤%熱穩定性%覈磁共振%雙酚A-雙苯併嗪%含DOPO的雙酚A-單苯併嗪
합성%취합%열은정성%핵자공진%쌍분A-쌍분병진%함DOPO적쌍분A-단분병진
synthesis%polymerization%thermostability%NMR%double benzoxazine based on bisphenol A%single benzoxazine containing DOPO based on bisphenol A
以双酚A、苯胺、多聚甲醛为原料,合成了双酚A-双苯并嗪(DBOZ),再用其与DOPO(9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物)反应,合成了含DOPO的双酚A-单苯并嗪(DBDO)。采用红外、核磁共振(氢谱核磁共振和碳谱核磁共振)等分析手段对DBOZ和DBDO的化学结构进行了表征;采用差示扫描量热仪对DBOZ和DBDO的固化特性进行研究,使用热重分析分析了所得聚苯并嗪的热稳定性。结果表明:在N2气氛中,DBOZ在205℃左右开环聚合,热分解温度为312℃,在373℃分解速度达到最快,在800℃时的残碳率为37.19%;在N2气氛中,DBDO的热分解温度为353℃,在443℃分解速度达到最快,在800℃时的残碳率为39.60%。
以雙酚A、苯胺、多聚甲醛為原料,閤成瞭雙酚A-雙苯併嗪(DBOZ),再用其與DOPO(9,10-二氫-9-氧雜-10-燐雜菲-10-氧化物)反應,閤成瞭含DOPO的雙酚A-單苯併嗪(DBDO)。採用紅外、覈磁共振(氫譜覈磁共振和碳譜覈磁共振)等分析手段對DBOZ和DBDO的化學結構進行瞭錶徵;採用差示掃描量熱儀對DBOZ和DBDO的固化特性進行研究,使用熱重分析分析瞭所得聚苯併嗪的熱穩定性。結果錶明:在N2氣氛中,DBOZ在205℃左右開環聚閤,熱分解溫度為312℃,在373℃分解速度達到最快,在800℃時的殘碳率為37.19%;在N2氣氛中,DBDO的熱分解溫度為353℃,在443℃分解速度達到最快,在800℃時的殘碳率為39.60%。
이쌍분A、분알、다취갑철위원료,합성료쌍분A-쌍분병진(DBOZ),재용기여DOPO(9,10-이경-9-양잡-10-린잡비-10-양화물)반응,합성료함DOPO적쌍분A-단분병진(DBDO)。채용홍외、핵자공진(경보핵자공진화탄보핵자공진)등분석수단대DBOZ화DBDO적화학결구진행료표정;채용차시소묘량열의대DBOZ화DBDO적고화특성진행연구,사용열중분석분석료소득취분병진적열은정성。결과표명:재N2기분중,DBOZ재205℃좌우개배취합,열분해온도위312℃,재373℃분해속도체도최쾌,재800℃시적잔탄솔위37.19%;재N2기분중,DBDO적열분해온도위353℃,재443℃분해속도체도최쾌,재800℃시적잔탄솔위39.60%。
Double benzoxazine based on bisphenol A(DBOZ)was synthesized from bisphenol A, aniline and paraformaldehyde, and the single benzoxazine containing DOPO based on bisphenol A(DBDO)was synthesized from DBOZ and DOPO. FT-IR, NMR (1H NMR and 13CNMR) were used to characterize the chemical structure of DBOZ and DBDO. Curing characteristics were studied with DSC and thermostability was studied with TG. In N2 atmosphere, the ring opening polymerization of DBOZ took place at about 205℃, and initial decomposition temperature was 312℃. At 373℃, the fastest decomposition was achieved. At 800℃, carbon residue was 37.19%. In N2 atmosphere, initial decomposition temperature of DBDO was 353℃. At 443℃, the fastest decomposition was achieved. At 800℃, carbon residue was 39.60%.