摘要
以SiCl4、三(2-羟乙基)异氰尿酸酯(赛克)和环氧氯丙烷为原料合成了有机硅酸酯阻燃剂三[2-三(二氯丙氧基)硅酰氧基乙基]异氰尿酸酯(简称赛克三硅酸二氯丙酯)。考察了溶剂种类、反应温度和反应物配比对合成反应的影响,得到了最佳的反应条件,并采用FTIR、1H NMR、TG-DTA分析及极限氧指数等技术表征了产物的结构和性能。最佳的反应条件为:n(SiCl4)∶n(环氧氯丙烷)∶n(赛克)=3∶9.8∶1,SiCl4先与环氧氯丙烷在50℃下反应2 h,再与赛克在90℃下反应9 h,最后与环氧氯丙烷于90℃下反应6 h。在此条件下,赛克三硅酸二氯丙酯的收率为93.7%。性能测试结果表明,该产物阻燃效能高,与聚氯乙烯的相容性好,适合用作聚氯乙烯等材料的阻燃剂。
An organic silicate flame retardant,isocyanurate tri（2-hydroxyethyl） ester three silicate dichloride propyl ester,was synthesized from tri（2-hydroxyethyl） isocyanurate（THEIC）,silicon tetrachloride and epichlorohydrin.The effects of solvent types,reaction temperature and reactant ratio on the synthesis were investigated.The product yield reached 93.7％ under the optimal conditions of n（SiCl4） ∶ n（epichlorohydrin） ∶ n（THEIC） 3 ∶ 9.8 ∶ 1,the first reaction of SiCl4 with epichlorohydrin at 50 ℃ for 2 h,the second reaction by adding THEIC at 90 ℃ for 9 h,and the third reaction by adding epichlorohydrin at 90 ℃ for 6 h.The structure and flame retardance of the product was characterized by means of FTIR,1H NMR,TG-DTA analysis and limiting oxygen index technique.The results showed that the product had the high flame retardance and could be used as a flame retardant for polyvinyl chloride.
出处
《石油化工》
CAS
CSCD
北大核心
2014年第6期693-697,共5页
Petrochemical Technology
