螺环磷-氮协同反应型阻燃剂的合成及在环氧树脂中的应用

Synthesis of Spiro-Phosphorus-Nitrogen Synergistic Flame Retardant and Its Application in Epoxy Resin

以三丙酮二胺、季戊四醇和三氯氧磷为原料,通过一锅法制备出一种新型环氧树脂反应型阻燃固化剂SPDPT,通过傅里叶变换红外光谱、核磁共振氢谱和磷谱,证明SPDPT制备成功。以4’,4-二氨基二苯砜(DDS)为共固化剂,共同固化环氧树脂制备了本征型阻燃环氧固化物(EP/DDS/SPDPT)。热重分析结果表明,SPDPT的加入能提高EP热固性材料燃烧后的残炭量。当磷质量分数为1.0%时,EP/DDS/SPDPT-4样品的LOI值为26.4%,UL94达到V-0级。在环氧固化物中,其拉伸强度最高达到了37.2 MPa,弯曲强度最高达到了63.8 MPa,冲击强度最高达到了21.6 kJ/m^2。

A novel epoxy resin reactive flame retardant curing agent SPDPT was prepared by one-pot method using triacetone diamine,pentaerythritol and phosphorus oxychloride as raw material.The preparation of SPDPT was proved by Fourier transform infrared spectroscopy,nuclear magnetic resonance spectroscopy and phosphorus spectroscopy.The intrinsic flame retardant epoxy cured product(EP/DDS/SPDPT)was prepared by co-curing epoxy resin with 4’,4-diaminodiphenyl sulfone(DDS)as co-curing agent.Results of TG show that the addition of SPDPT can increase the amount of carbon residue after burning of EP thermosetting materials.When the mass fraction of phosphorus is 1.0%,the LOI value of the EP/DDS/SPDPT-4 sample is 26.4%,and the UL94 reaches the V-0 level.In the epoxy cured product,the tensile strength rises up to 37.2 MPa,the bending strength reaches 63.8 MPa,and the impact strength is 21.6 kJ/m^2.