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以甲基膦酸二甲酯(DMMP)和乙二醇(EG)为原料,离子液体[Bmim]BF4与对甲苯磺酸(p-TSA)为协同催化剂,合成了一种阻燃剂聚甲基膦酸乙二醇酯。通过正交实验L9(33),确定最佳合成条件为:n(DMMP)∶n(EG)=1∶1;催化剂总用量为DMMP物质的量的3%,其中[Bmim]BF4占1%,p-TSA占2%;反应温度为155~170℃;反应时间为4 h。产物为淡黄色透明黏稠液体,酸值370 mg KOH/g。用红外光谱表征了产品结构;用液质分析了产品组成为十几种不同程度的乙二醇甲基膦酸二甲酯聚合物;用气质分析了副产物组成主要为甲醇、甲醚、乙二醇单甲醚、乙二醇二甲醚和二缩乙二醇。
A new kind of flame retardant Polymethylmethacrylate (PMMA) and ethylene glycol (EG) was synthesized by the reaction of ionic liquid [Bmim] BF4 and p-toluenesulfonic acid Ethylene phosphonate. The optimal synthesis conditions were as follows: n (DMMP): n (EG) = 1: 1; the total amount of catalyst was 3% of the amount of DMMP substance, and [Bmim] BF4 accounted for 1% , p-TSA accounted for 2%; reaction temperature was 155 ~ 170 ℃; reaction time was 4 h. The product is a pale yellow transparent viscous liquid with an acid value of 370 mg KOH / g. The structure of the product was characterized by FT-IR. The product composition was analyzed by liquid chromatography for a dozen of ethylene glycol methyl-methyl-phosphonate polymers with different degrees of toxicity. The main components of by-products were methanol, methyl ether and ethyl acetate Glycol monomethyl ether, ethylene glycol dimethyl ether and ethylene glycol.