新型耐热苯并噁嗪的制备与性能表征  

Preparation and Characterization of A New Type of Heat Resistant Benzoxazine

作　　者：王钊 高行[1,2,3] 张金枝[1,2,3] 柴仕淦 邹其超[1,2,3] WANG Zhao GAO Hang ZHANG Jin-zhi CHAI Shi-gan ZOU Qi-chao(Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials, Key Laboratory for the Synthesis and Application of Organic Functional Molecules Ministry of Education, College of Chemisty and Chemical Engineering Hubei University, Wuhan 430062, Chin)

机构地区：[1]有机化工新材料湖北省协同创新中心 [2]有机功能高分子合成和应用教育部重点实验室 [3]湖北大学化学化工学院,武汉430062

出　　处：《胶体与聚合物》2016年第3期118-121,共4页Chinese Journal of Colloid & Polymer

摘　　要：院采用对羟基苯甲酸丁酯,甲醛和烯丙基胺为原料合成了含双键的苯并噁嗪(BZ),并与9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)反应,最终合成含磷的苯并噁嗪(DOPO-BZ)。通过红外光谱,液质联用,核磁共振等技术对BZ、DOPO-BZ进行了结构表征确定了目标产物;采用差示扫描量热技术对产物的固化过程及聚合物的结构进行了表征。结果表明:BZ在高温下为两步固化,即先发生噁嗪环开环反应,而后发生双键聚合反应;DOPO-BZ则为一步噁嗪环开环固化反应;热失重结果表明PBZ分子链中引入含磷的DOPO刚性基团后,其耐热性显著得到提高。Benzoxazine with double bond（BZ） is synthesized by butyl parahydroxybenzoate,formaldehyde,and allyl amine,then phosphorous-containing benzoxazine（DOPO-BZ） is obtained by BZ and9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide（DOPO）.The structures of BZ and DOPO-BZ are characterized using Fourier transform infrared spectroscopy（FTIR）,liquid chromatograph-mass spectroscopy（LC-MS）,proton magnetic resonance（~1H-NMR）,and the curing behavior of the products and the structure of the polymer are characterized by differential scanning calorimetry（DSC）.The results reveal that BZ shows a two-step curing at high temperature,namely ring-opening raction of BZ and polrmerization of double bond afterwards;DOPO-BZ presents a one-step ring-opening curing,introduction of DOPO exerts a remarkable influence on the curing progress.TGA shows that the thermostability of PBZ is significantly improved with the introduction of huge rigid phosphorous-containing DOPO.

关 键 词：院DOPO 苯并噁嗪 烯丙基胺 合成 

分 类 号：O634[理学—高分子化学]