反应型阻燃剂THPP的制备及其在PU硬泡中的应用  

The Synthesis of a Reactive Phosphorous Flame-Retardant and Its Application in the Rigid Polyurethane Foam

作　　者：李马刚[1,2] 李其峰[2] 王军威[2] 殷宁[2] 亢茂青[2] 沈劲松 

机构地区：[1]中国科学院大学,北京100049 [2]中国科学院山西煤炭化学研究所,太原030001 [3]靖江市晨阳化工有限公司,江苏泰州214500

出　　处：《聚氨酯工业》2015年第6期12-15,共4页Polyurethane Industry

摘　　要：以三氯氧磷(POCl_3)和间苯二酚(RC)为原料,制备了含磷反应型阻燃剂磷酸三(间羟基)苯酯(THPP);考察了反应温度、反应物摩尔比、缚酸剂三乙胺(TEA)用量和反应时间对THPP产率的影响;利用凝胶渗透液相色谱(GPC)和热失重分析(TGA)对THPP进行了分析表征;并将THPP应用于聚氨酯(PU)硬泡中。结果表明,合成的化合物为目标产物THPP,且THPP具有良好的热稳定性;当n(POCl_3)∶n(RC)∶n(TEA)=1∶2.5∶2.5、45℃反应225 min时,THPP收率可达86.0%;与空白PU硬泡样品相比,添加10份THPP的PU硬泡样品的极限氧指数从19.8%提高到21.5%,残炭率(600℃)从19.7%提高到25.0%。The reactive flame-retardant tris-（ m-hydroxy phenyl） phosphate （ THPP ） was synthesized by one- step method from phosphorus oxychloride and resorcinol as main raw materials. The influence of the reaction tem- perature, mole ratio of reactants, dosage of trimethylamine and reaction time on the yield of THPP were investigated. THPP was analyzed and characterized by GPC and TGA, then was added in rigid polyurethane foam. The re- suits showed that the synthetic compound was the target product THPP, and the thermal stability of THPP was good. When the molar ratio of phosphorus oxychloride, resorcinol and trimethylamine was 1：2. 5：2. 5 and the reac- tion was conducted under 45℃ for 225 min, the yield of THPP could reach to 86. 0%. Compared with the blank sample of rigid polyurethane foam, the limiting oxygen index of the samples with adding 10 parts THPP increased from 19.8% of the blank sample to 21.5%, the carbon residue rate at 600℃ enhanced from 19.7% to 25.0%.

关 键 词：反应型阻燃剂 磷酸三(间羟基)苯酯 聚氨酯 硬质泡沫塑料 

分 类 号：TQ314.248[化学工程—高聚物工业]