广西师范学院学报(自然科学版)
廣西師範學院學報(自然科學版)
엄서사범학원학보(자연과학판)
JOURNAL OF GUANGXI TEACHERS EDUCATION UNIVERSITY(NATURAL SCIENCE EDITION)
2014年
3期
43-47,56
,共6页
蒋玉华%朱永飞%程马力%于淑娟
蔣玉華%硃永飛%程馬力%于淑娟
장옥화%주영비%정마력%우숙연
苯并噁嗪%氰基%热稳定性
苯併噁嗪%氰基%熱穩定性
분병오진%청기%열은정성
benzoxazine%nitrile group%thermal stability
以4-氰基苯酚、苯胺、多聚甲醛为起始原料,以甲苯为溶剂制备了苯并噁嗪中间体.用 FTIR、1 HNMR和13 CNMR对苯并噁嗪中间体进行了表征,同时,用 DSC 对其固化行为进行表征.通过 TGA 对聚苯并噁嗪的热稳定性进行了测试.DSC 研究结果表明:苯并噁嗪中间体的熔融温度为117.90℃,开环聚合的起始温度为225.00℃,固化峰值温度为232.10℃,低于类似结构的苯酚/苯胺型苯并噁嗪.TGA 研究表明:聚苯并噁嗪5%热失重温度为302.26℃,10%热失重温度为351.85℃,最大失重速率温度为433.91℃,残炭率为55.63%.与其他类似结构的苯并噁嗪相比,氰基的引入使其固化物的残炭率和热稳定性明显提高.
以4-氰基苯酚、苯胺、多聚甲醛為起始原料,以甲苯為溶劑製備瞭苯併噁嗪中間體.用 FTIR、1 HNMR和13 CNMR對苯併噁嗪中間體進行瞭錶徵,同時,用 DSC 對其固化行為進行錶徵.通過 TGA 對聚苯併噁嗪的熱穩定性進行瞭測試.DSC 研究結果錶明:苯併噁嗪中間體的鎔融溫度為117.90℃,開環聚閤的起始溫度為225.00℃,固化峰值溫度為232.10℃,低于類似結構的苯酚/苯胺型苯併噁嗪.TGA 研究錶明:聚苯併噁嗪5%熱失重溫度為302.26℃,10%熱失重溫度為351.85℃,最大失重速率溫度為433.91℃,殘炭率為55.63%.與其他類似結構的苯併噁嗪相比,氰基的引入使其固化物的殘炭率和熱穩定性明顯提高.
이4-청기분분、분알、다취갑철위기시원료,이갑분위용제제비료분병오진중간체.용 FTIR、1 HNMR화13 CNMR대분병오진중간체진행료표정,동시,용 DSC 대기고화행위진행표정.통과 TGA 대취분병오진적열은정성진행료측시.DSC 연구결과표명:분병오진중간체적용융온도위117.90℃,개배취합적기시온도위225.00℃,고화봉치온도위232.10℃,저우유사결구적분분/분알형분병오진.TGA 연구표명:취분병오진5%열실중온도위302.26℃,10%열실중온도위351.85℃,최대실중속솔온도위433.91℃,잔탄솔위55.63%.여기타유사결구적분병오진상비,청기적인입사기고화물적잔탄솔화열은정성명현제고.
In this paper,a new type of benzoxazine monomer containing the nitrile group was syn-thesized by 4-cyano phenol,aniline and paraformaldehyde in a solvent of toluene.The structure of the monomer was investigated by FTIR、1 H-NMR、13 C-NMR.At the same time,the curing behavior was researched by DSC.The thermal stabilities of the polybenzoxazine were investigated by thermogravim-etric analysis (TGA).The results of DSC showed that melting temperature of the monomer was 117.90℃,the polymerization temperature was 232.10℃,which was lower than the ordinary benzox-azine based on phenol and aniline.The results of TG showed that 5% and 10% weight loss of poly-benzoxazine were at 302.62℃ and 351.85℃ respectively.The temperature of maximum weight loss rate was 433.91℃,the char yield of 800℃ was 55.63%.Compared with other benzoxazines with the similar structure,the introduction of nitrile group increased the char yield and the thermal stability of the polybenzoxazine.