金刚烷基磺酸盐阻燃剂的制备及在聚碳酸酯中的应用

Synthesis of Aromatous Sulfonate Flame Retardant Based on Adamantane and Its Application to Polycarbonate

以1-溴金刚烷为原料,与苯发生傅克酰基化反应制得1,3,5,7-四苯基金刚烷,再与氯磺酸磺化制得1,3,5,7-四(苯基-4-磺酰氯)金刚烷,最后经过水解和中和反应制得目标产物1,3,5,7-四(苯基-4-磺酸钠)金刚烷阻燃剂(FR-A)。所有化合物均经傅里叶变换红外光谱、核磁共振、元素分析确证。将FR-A与聚碳酸酯(PC)共混,通过氧指数法和垂直燃烧测试法(UL94)测试了其阻燃性能,采用热重分析研究其热降解行为。结果表明,FR-A加入量为0.08%(质量分数)时,其阻燃效果明显提高,并且通过UL-94 V-0级实验。结合热重分析和差示扫描量热数据分析,添加阻燃剂后质量损失的起始温度和最大质量损失速率峰的发生温度均有所提高,产热量减少,具有较好的阻燃性能。

A sulfonate flame retardant,1,3,5,7-tetrakis( phenyl-4-sodium sulfonate) adamantane( FR-A),was synthesized from 1-bromoadamantane in sequential four-step reactions involving Fiedel-Crafts phenylation obtaining 1,3,5,7-tetraphenyladamantane,sulphonation from chlorosulfonic acid obtaining 1,3,5,7-tetrakis( phenyl-4-sulfonyl chloride),hydrolysis,and neutralization. The success of synthesis was confirmed by FT-IR spectra,1H-NMR spectra,elemental analyses. The effect of FR-A on the flame retardancy of polycarbonate( PC) was studied. Limiting oxygen index( LOI) and thermogravimetric analysis( TGA) show that this novel sulfonate flame retardant has effective flame retardancy on polycarbonate( PC). With small amount( 0. 08%) of FR-A,the flame retardancy of PC is improved obviously,which gets to UL 94 V-0 rating. TGA and DTG curves demonstrate that after adding FR-A,the initial temperature and the maximum peak temperature of mass loss increase and the heat production reduces,indicating that FR-A has excellent fire-retardant properties.