摘要
以双酚A、三氯氧磷、苯酚等廉价原料,通过两步反应合成双酚-A双(磷酸二苯酯)阻燃剂,总收率95%。采用红外光谱、核磁共振氢谱、质谱、元素分析等对产物结构进行表征。研究反应原料配比、催化剂用量、反应温度、反应时间等因素对收率的影响。适宜反应条件为:以氯化镁为催化剂,n(双酚A)∶n(催化剂)∶n(三氯氧磷)∶n(苯酚)=1∶0.01∶4.0∶5.0,第一步反应温度控制在65℃,反应时间3h;第二步反应温度控制在120℃,反应时间12h;热失重分析(TGA)表明:合成的双酚-A双(磷酸二苯酯)阻燃剂起始分解温度为299.16℃,在299.16～386.66℃和386.66～439.16℃温区迅速炭化;阻燃剂在330℃失重1%,阻燃剂被加热到427.50℃时,炭残余量为46.26%,已经达到了塑料的加工温度要求;合成的双酚-A双(磷酸二苯酯)阻燃剂阻燃性能达到UL94V-0级。
The flame retardant, bisphenol-A Bis （dipenyl phosphate） was prepared from phospous oxychloride, bisphenol A and phenol by facile, high efficient and useful method consisting of two steps reactions. The overall yield was 95%. The product was characterized by FT-IR, MS-TOF, 1H NMR and elementary analysis. At the same time, the effects of material mole ratio, catalyst species and ratio, reaction temperature and time on the reaction were studied. The optimum ratios of reactants presented by experiments were n（bisphenol A） ： n（catalyst） ：n（phosphorus trichloride） ： n （phenol） = 1：0.01：4.0：5.0 via catalyst of MgC12. The optimized reaction was conducted at 65℃ for 3 hours in the first step reaction, and 120℃ for 12 hours in the final step reaction. The termogravimetry showed that the beginning temperature of the compound decomposition was above 299.16℃, and rapidly carbonized between 299.16℃ to 388.66℃ and 388.66 to 439.16℃. The char yield was about 46.26% at 427.50℃. which were adequate for plastic processing. The addition of BDP to ABS can increase the flame retardance of the ABS to UL94V-0 rating.
出处
《精细化工中间体》
CAS
2007年第4期59-62,共4页
Fine Chemical Intermediates
基金
公安部应用创新项目(2006YYCXWJXYXY094)。
关键词
阻燃剂
双酚-A双(磷酸二苯酯)
合成
flame retardant
bisphenol-A bis （dipenyl phosphate）
synthesis
