三(2-羟丙基)磷酸酯的合成

Synthesis of Tris (2-hydroxypropyl) phosphate

以磷酸和环氧丙烷为原料,Et3NHCl-Al Cl_3离子液体为催化剂合成反应型阻燃剂——三(2-羟丙基)磷酸酯。采用红外、核磁、质谱对其结构进行了表征。考察了催化剂种类及用量、物料比〔n(H3PO4)∶n(环氧丙烷)〕、反应时间和反应温度等因素对反应的影响。得到最佳反应条件为:n(H3PO4)∶n(环氧丙烷)=1.0∶3.2,反应温度为90℃,反应时间为3 h,Et3NHCl-Al Cl_3用量为3%(以磷酸和环氧丙烷的总质量为基准,下同),在该条件下三(2-羟丙基)磷酸酯收率可达92.8%。热重分析表明,温度600℃时,三(2-羟丙基)磷酸酯的残炭率为16.66%,其稳定性符合材料加工要求,阻燃性能优良。

A reactive flame retardant, tris(2-hydroxypropyl) phosphate was synthesized using phosphoric acid and propylene oxide as raw materials in the presence of a catalytic amount of Et3 NHCl-AlCl3 ionic liquid. Its structure was characterized by FTIR, nuclear magnetic resonance and mass spectrometry. The effects of the type and amount of catalyst, molar ratio of phosphoric acid to propylene oxide, reaction time and reaction temperature on the yield of the product were studied. The results showed that the optimum conditions were as follows: n(phosphoric acid): n(propylene oxide)=1.0 : 3.2, reaction temperature 90 ℃, reaction time 3 h, catalyst dosage 3%(based on the total mass of phosphoric acid and propylene oxide, the same below). Under these conditions, the yield of tris(2-hydroxypropyl) phosphate reached 92.8%. The performances of the product were excellent. The thermogravimetric analysis revealed that carbon yield of tris(2-hydroxypropyl) phosphate was 16.66% at 600 ℃, its stability met the material processing requirements.