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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。
In the hospital, double bond benzoxazine (BZ) was synthesized from butylparaben, formaldehyde and allylamine and reacted with 9,10-dihydro-9-oxa-10-phosphaphenanthrene -10-oxide (DOPO) reaction, the final synthesis of phosphorus-containing benzoxazine (DOPO-BZ). The structures of BZ and DOPO-BZ were characterized by FTIR, LC / MS and NMR. The products were characterized by differential scanning calorimetry and their structures were characterized. The results showed that BZ was cured in two steps at high temperature, that is, the ring opening reaction of oxazine ring occurred first, then the double bond polymerization occurred. DOPO-BZ ring opening reaction of oxazine ring in one step. In the introduction of phosphorus-containing DOPO rigid group, the heat resistance was significantly improved.