含磷环氧树脂固化剂的合成表征与环氧树脂复合材料阻燃性能的研究  

Synthesis and characterization of phosphorous-containg epoxy resin curing agent and flame retarding performance of epoxy resin composite material

作　　者：王刚[1] 唐禹[1] 何冬青[1] 朱思巧 梁兵[1] 

机构地区：[1]沈阳化工大学材料科学与工程学院,沈阳110142

出　　处：《功能材料》2016年第7期7135-7139,7144,共6页Journal of Functional Materials

基　　金：国家科技支撑计划资助项目(2012BAB06B03);国家国际科技合作与交流专项资助项目(2013DFA51200);辽宁省高等学校创新团队资助项目(LT2012010)

摘　　要：以季戊四醇(PER)、三氯氧磷(POCl_3)和乙二胺(EDA)为原料合成了一种阻燃固化剂聚乙二胺季戊四醇螺磷酸酯(PES),并通过红外光谱(FT-IR),核磁共振(1 H NMR)、质谱(ESI-MS)和热重分析(TGA)对其结构和热性能进行了表征。并以PES和4,4-二氨基二苯砜(DDS)为固化剂,双酚A型环氧树脂(E-51)为基体树脂,制备了不同含磷量的阻燃环氧树脂复合材料。通过极限氧指数(LOI)和垂直燃烧(UL-94)实验表征了环氧树脂复合的阻燃性能,热重分析和扫描电镜研究了阻燃环氧树脂的热性能和残炭形貌。研究发现,随着磷含量增加,阻燃环氧树脂的初始分解温度逐渐降低,但与纯样相比,在600℃时的残炭量显著增加,且随着PES加入量的增大,SEM观察形成的炭层越致密。当磷含量为3.48%时,其LOI值可达28.9,并通过UL-94V0级测试,拉伸强度和冲击强度分别达到了62.76 MPa和6.81kJ/m^2,表明PES是一种良好的环氧树脂阻燃剂。With pentaerythritol（PER）,phosphorus oxychloride（POCl3）and ethylenediamine（EDA）as raw material synthesis a kind of flame retardant agent poly-ethylene diamine pentaerythritol screw phosphate（PES）,which the chemical structure and thermal properties were characterized by fourier transform infrared spectrum（FT-IR）,nuclear magnetic resonance（1 H NMR）,mass spectrometry（ESI-MS）and thermogravimetric analysis（TGA）.With PES and 4,4-diamino diphenyl sulfone（DDS）as curing agent,bisphenol A type epoxy resin（E-51）as the matrix resin prepared different phosphorus flame retardant epoxy resin composite material.The flame retardant properties of epoxy resin composite was characterized by limiting oxygen index（LOI）and vertical（UL-94）experimental characterization of the combustion,TGA and SEM would study the thermal properties and the epoxy resin carbon residue morphology.The study found that with the increase of phosphorus content,the initial decomposition temperature of flame retardant epoxy resin decreases gradually,but compared with the pure sample,the amount of residual carbon increased significantly at 600 ℃,and with the increase of PES addition amount,the formation of the carbon layer was dense.When the phosphorus content was 3.48%,and its LOI value was 28.9,and through the UL-94 test level V-0ranking,tensile strength and impact strength were 62.76 MPa and 6.81kJ/m2 respectively.It shows that PES was a kind of good flame retardant for epoxy resin.

关 键 词：环氧树脂 含磷固化剂 阻燃 力学性能 

分 类 号：TB324[一般工业技术—材料科学与工程] O627.51[理学—有机化学]