摘要
研究了以三氯氧磷、乙二醇、环氧氯丙烷为原料、TiCl4为催化剂、通过两步反应合成四(1,3-二氯-2-丙基)-1,2-亚乙基二磷酸酯阻燃剂的方法,对反应条件进行了优化。结果表明,当原料摩尔配比n乙二醇:n三氯氧磷:n环氧氯丙烷为1:2.3:4.2,反应温度分别为15~18℃、50~60℃,反应时间分别为3.5h、4h,催化剂用量为0.6%(与原料总量之比),制得的目标产物最好,以乙二醇计产率达92.3%。通过红外光谱和磷含量分析对产物进行了表征。用其制阻燃聚氨酯软泡,具有较好的阻燃效果。
The flame - retardant 1,2-ethylene bis [bis ( 1,3-dichloro-2-propyl ) phosphate ] was synthesized with phosphorus trichloride, glycol, epichlorohydrin and titanium tetrachloride as catalyst through two steps. The reaction conditions of each step were optimized. The optimal reaction condition were as follows, molar ratio of glycol, phosphorus trichloride ,epichlorohydrin was 1:2.3:4.2 ; reaction temperature of each step was 15 - 18℃ and 50 60℃, reaction time of each step was 3.5h and 4h. The optimal condition of the amount of catalyst is 0.6% ( percent of raw material). The yield reached 92.3 % ( measured by glycol). The product was characterized by IR and determination of the phosphorus content. The obtained phosphate was used to soft polyurethane foam and get satisfactory result.
出处
《聚氨酯工业》
2006年第2期22-24,共3页
Polyurethane Industry