以季戊四醇(PER)、三氯氧磷(POCl3)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-94 V0级测试,拉伸强度和冲击强度分别达到了62．76 MPa和6．81 kJ/m2,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 thermogravime-tric analysis (TGA).With PES and 4,4-diamino diphenyl sulfone (DDS)as curing agent,bisphenol A type ep-oxy resin (E-51)as the matrix resin prepared different phosphorus flame retardant epoxy resin composite mate-rial.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-0 ranking,tensile strength and impact strength were 62.76 MPa and 6.81 kJ/m2 respectively.It shows that PES was a kind of good flame retardant for epoxy resin.
参考文献
| [1] | 田秀娟;王忠卫;于青;高军.含磷阻燃剂的合成及对环氧树脂阻燃性能的影响[J].高分子材料科学与工程,2014(8):31-36. |
| [2] | Jirasutsakul, I.;Paosawatyanyong, B.;Bhanthumnavin, W..Aromatic phosphorodiamidate curing agent for epoxy resin coating with flame-retarding properties[J].Progress in Organic Coatings: An International Review Journal,201312(12):1738-1746. |
| [3] | Qiang Lv;Jian-Qian Huang;Ming-Jim Chen.An Effective Flame Retardant and Smoke Suppression Oligomer for Epoxy Resin[J].Industrial & Engineering Chemistry Research,201327(27):9397-9404. |
| [4] | Zhan, J;Song, L;Nie, SB;Hu, YA.Combustion properties and thermal degradation behavior of polylactide with an effective intumescent flame retardant[J].Polymer Degradation and Stability,20093(3):291-296. |
| [5] | Chengwu Yang;Guozheng Liang;Aijuan Gu.Flame Retardancy and Mechanism of Bismaleimide Resins Based on a Unique inorganic-Organic Hybridized Intumescent Flame Retardant[J].Industrial & Engineering Chemistry Research,201343(43):15075-15087. |
| [6] | Chen, DQ;Wang, YZ;Hu, XP;Wang, DY;Qu, MH;Yang, B.Flame-retardant and anti-dripping effects of a novel char-forming flame retardant for the treatment of poly(ethylene terephthalate) fabrics[J].Polymer Degradation and Stability,20052(2):349-356. |
| [7] | Haiwang Xiang;Caiying Sun;Dawei Jiang.A Novel Halogen-Free Intumescent Flame Retardant Containing Phosphorus and Nitrogen and Its Application in Polypropylene Systems[J].Journal of Vinyl & Additive Technology,20104(4):261-271. |
| [8] | Haiyun Ma;Lifang Tong;Zhongbin Xu;Zhengping Fang;Yongming Jin;Fengzhu Lu.A novel intumescent flame retardant: Synthesis and application in ABS copolymer[J].Polymer Degradation and Stability,20074(4):720-726. |
| [9] | Shiqiang Song;Jiajun Ma;Ke Cao;Guanjun Chang;Yawen Huang;Junxiao Yang.Synthesis of a novel dicyclic silicon-/phosphorus hybrid and its performance on flame retardancy of epoxy resin[J].Polymer Degradation and Stability,2014:43-52. |
| [10] | Xiaodong Qian;Lei Song;Saihua Jiang.Novel Flame Retardants Containing 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and Unsaturated Bonds: Synthesis, Characterization, and Application in the Flame Retardancy of Epoxy Acrylates[J].Industrial & Engineering Chemistry Research,201322(22):7307-7315. |
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