含硅磷腈阻燃剂SCP-DOPO改性环氧树脂制备及性能

Preparation and properties of SCP-DOPO modified epoxy resin containing silicone phosphonitrile flame retardant

摘要:

以六氯三聚磷腈、对羟基苯甲醛、对氨基苯甲酸、9, 10-二氢-9-氧杂-10-磷杂菲-10-氧化物和三苯基硅醇为原料，合成了一种含硅磷腈阻燃剂（SCP-DOPO）。采用FTIR、1HNMR和31PNMR对其结构进行了表征，并且探究了SCP-DOPO用量对环氧树脂热稳定性、阻燃性能及粘接性能的影响。结果表明，当SCP-DOPO添加量为4%和8%时，改性环氧树脂的剥离强度分别为3.06 kN/m和2.64 kN/m，优于纯环氧树脂。当SCP-DOPO添加量为8%和12%时，改性环氧树脂对应残炭的石墨化程度提高，且垂直燃烧（UL-94）测试均为V-0等级，极限氧指数（LOI）分别达到31.1%和31.6%。拉曼测试结果进一步表明其具有良好的成炭性，故此改性环氧树脂具有优良的阻燃性能。

Abstract:

A silicon-containing phosphonitrile flame retardant (SCP-DOPO) was synthesized from hexachlorotrisphosphonitrile, p-hydroxybenzaldehyde, p-aminobenzoic acid, 9, 10-dihydro-9-oxa-10-phosphame-10-oxide (DOPO) and triphenylsilanol. The structures were characterized by FTIR, 1HNMR and 31PNMR, and the effects of SCP-DOPO dosage on the bond performance, thermal stability and flame retardancy of epoxy resin were also investigated. The results showed that the peel strength of the modified epoxy resin was 3.06 kN/m and 2.64 kN/m, respectively, when the dosage of SCP-DOPO was 4% and 8%, which was superior to that of the pure epoxy resin. When the addition of SCP-DOPO was 8% and 12%, the degree of graphitization of the modified epoxy resin corresponding to the residual carbon was increased, and the vertical combustion (UL-94) test was V-0 grade, and the limiting oxygen index (LOI) reached 31.1% and 31.6%, respectively. The Raman test results further showed that it has good charring properties, so the modified epoxy resin has excellent flame retardant properties.