摘要
以季戊四醇和40%氢溴酸溶液为原料,冰醋酸为催化剂,经取代反应、减压分离、纯化和干燥等步骤合成了具有优良性能的反应型阻燃剂2,2二(溴甲基)1,3丙二醇,以季戊四醇计,产品收率为80.8%。实验确定了氢溴酸与季戊四醇的最佳摩尔比为2.5∶1,最佳反应时间为6~8h,最佳反应温度为回流温度。先用等体积的甲苯和水混合物分离合成产物,再用热水重结晶进行纯化。经元素分析、熔点测定和红外光谱分析予以确证。
Bis(bromomethyl) 1,3 propanediol as a good reaction type fire retardant was synthesized by some processes such as replacement reaction, decompression separation, purification and drying from pentaerythrite and 40% hydrobromic acid solution in catalysis of glacial acetic acid, with a yield of 80.8%. It was shown that the optimum molar ratio between hydrobromic acid and pentaerythrite was 2.5 to 1 for 6 to 8h of optimum reaction time and reflux temperature as optimum reaction temperature. The synthesized product was separated using a mixture of toluene and water(equal volume)and then purified by recrystallization using hot water. The results of elementary analysis, m.p. determination and IR spectrometry indicated that the synthesized product was 2,2 bis(bromomethyl) 1,3 propanediol.
出处
《精细化工》
EI
CAS
CSCD
北大核心
1998年第4期36-38,共3页
Fine Chemicals
关键词
丙二醇
合成
二溴甲基
阻燃剂
bis(bromomethyl) 1,3 propanediol, fire retardant, pentaerythrite, hydrobromic acid, synthesis