微波法合成DOPO基反应型含磷阻燃剂  

Microwave-assisted synthesis of phosphorus-containing reactive flame retardants

作　　者：吴申德 张胜[1] 谷晓昱[1] 姜鹏[1] 扈中武[1] 赵倩[1] 

机构地区：[1]北京化工大学碳纤维及功能高分子教育部重点实验室,北京100029

出　　处：《化工新型材料》2015年第7期188-190,共3页New Chemical Materials

摘　　要：以对苯醌和9,10-二氢-9氧杂-10-磷杂菲-10-氧化物(DOPO)为原料,采用微波法合成了10-(2,5-二羟基苯基)-9,10-二氢-9氧杂-10-磷杂菲-10-氧化物(ODOPB)。通过核磁共振氢谱以及红外光谱对其结构进行了表征。讨论了投料比、反应时间以及反应温度对ODOPB产率的影响。确定了优化的合成工艺条件,即反应物配比n(苯醌)∶n(DOPO)=0.21∶1,反应温度为54℃,微波辐射功率为300W,辐射时间为5min。结果显示该条件下ODOPB产率为96.5%,产物的初始热分解温度为278℃,800℃残炭量达到33.5%;当产物添加量为15%时,LOI增加6个单位。10-（2,5-dihydroxyphenyl）-9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide（ODOPB）was prepared by microwave-assisted synthesis.The structure of product was characterized by NMR and FT-IR.The optimal synthesis conditions were determined after a series of experiments,that were n（Benzoquinone）∶n（DOPO）=0.21∶1;the reaction temperature 54℃ and the irradiation time 5minutes under 300 W microwave power.The results showed that the yield of product reached 96.5%.The synthesized derivative had a initial decomposition temperature of 278℃,and carbon residue of33.54% at 800℃.LOI increased 6percent when the product addition was 15 percent.

关 键 词：微波法 含磷阻燃剂 DOPO 

分 类 号：TQ314.248[化学工程—高聚物工业]