摘要
以苯基磷酰二氯和间苯二酚为原料合成了含磷阻燃剂苯磷酸二(间苯二酚)酯(BPHPPO),将其与顺丁烯二酸酐、邻苯二甲酸酐、1,2-丙二醇进行共聚,得到主链含磷的反应型阻燃不饱和聚酯(UPR)。当UPR固化物中BPHPPO的质量分数为18%时,UPR固化物的极限需氧指数为30,阻燃效果达到美国UL94-V0级标准。热重分析结果表明,当UPR固化物中BPHPPO的质量分数从0增至18%时,UPR的5%失重温度由275.5℃降至248.0℃,P—O—C键的提前分解促使磷酸类物质的生成并有效阻碍了UPR的进一步分解,600℃时的残炭量由0增至4.6%。用差示扫描量热仪测试了UPR的固化过程,以Kamal模型计算出UPR固化动力学参数,当UPR固化物中BPHPPO的质量分数由0增至18%时,固化反应活化能由46.5kJ/mol增至262.9kJ/mol。
A novel phosphorus-containing flame-retardant unsaturated polyester resin （UPR） was prepared by introducing a reactive flame retardant, bis-phenoxy （3-hydroxy） phenyl phosphine oxide （BPHPPO）, into the polyester by its copolymerization with maleic anhydride, phthalic anhydride and propylene glycol. BPHPPO was synthesized from phenyl phosphonic dichloride and resorcinol. The cured UPR reached American UL94-V0 standard rating and limiting oxygen index of 30 with BPHPPO content of as low as 18 % （ mass fraction）. Thermal properties of UPR were studied by means of TG and DTG. Decomposition temperature of 5% mass loss dropped from 275.5 ℃ to 248.0 ℃ with increase of BPHPPO mass fraction from 0 to 18 %. However, formation of phosphorus-containing acid from decomposition of P--O--C bonds inhibited effectively further decomposition of polyester. The char residue increased from 0 to 4.6% at 600℃. Curing kinetic parameters of UPR were calculated from Kamal＇ s equation by using DSC. Apparent activation energy increased from 46.5 kJ/mol to 262.9 kJ/mol with increasing of mass fraction of BPHPPO in UPR from 0 to 18 %.
出处
《石油化工》
CAS
CSCD
北大核心
2009年第5期515-520,共6页
Petrochemical Technology
基金
广州市花都区科技计划项目(HD07GY018)
关键词
反应型含磷不饱和聚酯
苯磷酸二(间苯二酚)酯
阻燃剂
固化动力学
reactive phosphorus-containing unsaturated polyester resin
bis-phenoxy （3-hydrogen） phenyl phosphine oxide
flame retardant
curing kinetics
