含季戊四醇磷酸酯阻燃剂的合成与表征

Synthesis,characterization and thermal stability of flame retardant containing pentaerythrityl phosphate

采用1-氧代-4-羟甲基-2,6,7-三氧杂-1-磷杂双环[2.2.2]辛烷(PEPA)、三氯氧磷、双酚A和双酚S为反应物,合成了两个新型添加型阻燃剂:双酚A双[二(1-氧代-1-磷杂-2,6,7-三氧杂双环辛烷-4-亚甲基)]磷酸酯(BAPP)和双酚S双[二(1-氧代-1-磷杂-2,6,7-三氧杂双环辛烷-4-亚甲基)]磷酸酯(BSPP),通过元素分析、FT-IR和1H NMR等表征了标题化合物的结构,结果表明,所合成的标题化合物的结构与预期一致。热失重分析结果证明,BAPP和BSPP质量损失5%(wt)时的温度分别为343.6℃和352.3℃,600℃残余量分别达46.6%和55.5%,具有较高的热稳定性和结炭性能。阻燃性能实验证明,E-51环氧树脂中分别添加质量分数为18.2%(wt)的BAPP和BSPP时,极限氧指数分别为32.2%和31.8%,均能达到UL 94 V-0级。

Two novel phosphorus-containing flame retardant, bisphenol A bis [ di （2,6,7-trioxa-l-phospha-bicyelo [ 2. 2. 2 ]-octane-1- oxo-4-hydroxymethyl） ] phosphate （BAPP） and bisphenol S his [ di （ 2,6,7-trioxa-l-phosphabicyclo [ 2. 2. 2 ] -octane-l-oxo-4-hydroxy- methyl ） ] phosphate （BSPP） were synthesized from 1 -oxo-4-hydroxymethyl-2,6,7-trioxa-1 -phosphabieyclo [ 2.2.2 ] octane （ PEPA ）., phosphorus oxychloride, bisphenol A and bisphenol IS. The title compounds were characterized by elemental analysis, FT-IR, and 1H NMR. Results showed that the structure of the title compounds were in consistent with the expected one. An investigation on thermal stability of BAPP and BSPP,which had been examined using thermogravimetry （TG）, showed that the mass loss of 5% （wt）was 343.6℃ and 352. 3℃ ,respectively and residue at 600℃ was as high as 46.6% and 55.5% ,respectively. The limiting oxygen index （LOI） value could reach 32.2% and 31.8% ,respectively and the flame retardaney were UL 94 V-0 when the mass fraction of the BAPP and BSPP flame retardant in the E-51 epoxy resin was 18.2%.