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以3-氨基苯酚、戊二醛及9,10-2H-9-氧杂-10-磷杂菲-10-氧化物(DOPO)为原料,制备了一种磷氮阻燃剂1,5-双(3-羟基苯氨基)-1,5-双{二苯并[c,e][1,2]氧杂膦-6-氧化物}戊烷(GAP-DOPO),对中间体1,5-双(3-羟基苯基亚胺基)戊烷(GAP)和GAP-DOPO的物料配比、溶剂用量、反应温度和反应时间进行了单因素考察,GAPDOPO的最佳合成条件为:n(GAP)∶n(DOPO)=1.0∶2.1,溶剂用量为GAP质量的10倍,反应温度为90℃,反应时间为6 h。通过FTIR、~1HNMR与TGA对阻燃剂的结构及热性能进行了表征;将GAP-DOPO用于阻燃环氧树脂(E-51),制备了3种阻燃环氧树脂复合材料EP1、EP2和EP3,并用TGA、SEM对复合材料的热性能及残炭结构进行了表征,使用垂直燃烧测试仪对试样进行了燃烧测试。结果表明:当w(GAP-DOPO)=30%时,EP3可通过UL94 V-0级测试;TGA结果显示,在800℃(N_2氛围)下,EP3残炭率为21.5%,与纯环氧树脂的16.3%相比,提高了31.9%;SEM结果表明:阻燃剂的加入能够明显改善环氧树脂燃烧后残炭形貌,GAP-DOPO能够提高环氧树脂的阻燃性能。
Using 3-aminophenol, glutaraldehyde and 9,10-2H-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) as raw materials, Intermediate 1, bis (3-hydroxyphenylamino) -1,5-bis {dibenzo [c, e] [1,2] oxaphosphine-6-oxide} pentane (GAP-DOPO) The optimum conditions for the synthesis of GAPDOPO were as follows: the molar ratio of 5-bis (3-hydroxyphenylimino) pentane (GAP) to GAP-DOPO, the amount of solvent, the reaction temperature and the reaction time were investigated. (GAP): n (DOPO) = 1.0: 2.1, the amount of solvent was 10 times of the mass of GAP, the reaction temperature was 90 ℃ and the reaction time was 6 h. The structure and thermal properties of the flame retardant were characterized by FTIR, 1HNMR and TGA. Three flame retardant epoxy resin composites EP1 and EP1 were prepared by flame-retardant epoxy resin (E-51) with GAP-DOPO. EP2 and EP3. The thermal properties and residual carbon structure of the composites were characterized by TGA and SEM. The vertical burning tester was used to test the combustion of the samples. The results showed that EP3 passed the UL94 V-0 test when GAP-DOPO was 30%. The TGA results showed that the char yield of EP3 was 21.5% at 800 ℃ (N2 atmosphere) SEM results showed that the addition of flame retardant can significantly improve the morphology of the carbon residue after burning epoxy resin, GAP-DOPO can improve the flame retardancy of the epoxy resin.