端羟基聚丁二烯/环氧氯丙烷合成多羟基聚丁二烯的实验研究

Studies on the Hydroxyl-terminated Polybutadiene/Epichlorohydrin Synthesis of Polyhydroxylated Polybutadiene

在氢氧化钠碱性条件下,以端羟基聚丁二烯(HTPB)和环氧氯丙烷(ECH)为原料,四丁基溴化铵(TBAB)为催化剂,制得多羟基聚丁二烯(PHPB)。采用红外光谱(IR)、热重分析仪(TG)、核磁共振(1 H-MNR)对原料、中间产物和产物的结构和热稳定性进行了分析。通过产品的羟值、粘度和产率详细考察了反应温度、反应时间、原料配比、催化剂用量和氢氧化钠用量对PHPB合成的影响。结果表明,最适宜合成工艺条件为:反应温度为55℃,反应时间1.5h,n(HTPB)∶n(ECH)∶n(NaOH)∶n(TBAB)=1∶2.9∶3∶0.03。

Under the alkaline condition of sodium hydroxide,the polyhydroxylated polybutadiene （PHPB） was synthesized by hydroxyl tcrminated polybutadiene （HTPB） and epichlorohydrin （ECH）.Tetrabutyl ammonium bromide （TBAB） as the catalyst in this reaction.The structure and thermal stability of raw material,intermediate products and product were analyzed by Infrared spectroscopy （IR）,thermogravimetry （TG） and nuclear magnetic resonance （1 H-MNR）.The effect of reaction temperature,reaction time,raw material ratio,catalyst dosage and dosage of sodium hydroxide on the on the PHPB synthesis were investigated in detail by the hydroxyl value,viscosity and yield of the product.The result showed that the optimum synthesis conditions were as follows：reaction temperature was 55 ℃,reaction time was 1.5h,n（HTPB）∶n（ECH）∶n（NaOH）∶n（TBAB） =1 ∶2.9∶3∶ 0.03.