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支化3,3-二叠氮甲基环氧丁烷-四氢呋喃的合成及表征
引用本文:王娟,黄洪勇,杨建国,肖乐勤,周伟良.支化3,3-二叠氮甲基环氧丁烷-四氢呋喃的合成及表征[J].固体火箭技术,2017,40(5).
作者姓名:王娟  黄洪勇  杨建国  肖乐勤  周伟良
作者单位:1. 南京理工大学 化工学院,南京,210094;2. 中国航天科技集团公司八院806所,湖州,313002
摘    要:以3,3-叠氮甲基环氧丁烷-四氢呋喃(PBT)为起始聚醚,三官能度的支化单元为引发剂,在催化剂的作用下,通过亲核加成反应合成一种具有新型支化结构的PBT(B-PBT)。采用FTIR、~1H-NMR、粘度测试、DSC、TG和拉伸测试,对目标产物的结构、粘度特征、热稳定性以及力学性能进行表征。结果表明,所合成的目标产物为具有支化结构的叠氮缩水甘油醚;B-PBT的粘度(15 000 mPa·s/50℃)明显低于PBT(23 828 mPa·s/50℃);引入支化单元后,B-PBT热稳定性仍保持良好,放热达到1481 J/g;产物热分解分为两个阶段,即叠氮基热分解、支化单元以及主链的断裂和小分子的热解;制备的B-PBT弹性体拉伸强度达到5.29 MPa,延伸率达到516.42%,力学性能良好。

关 键 词:3  3-二叠氮甲基环氧丁烷-四氢呋喃  支化  粘度  热稳定性

Synthesis and characterization of branched 3,3-butylene azidomethyl-tetrahydrofuran
WANG Juan,HUANG Hong-yong,YANG Jian-guo,XIAO Le-qin,ZHOU Wei-liang.Synthesis and characterization of branched 3,3-butylene azidomethyl-tetrahydrofuran[J].Journal of Solid Rocket Technology,2017,40(5).
Authors:WANG Juan  HUANG Hong-yong  YANG Jian-guo  XIAO Le-qin  ZHOU Wei-liang
Abstract:Using 3,3-Bis( azidomethyl) oxetane/Tetrahydrofuran ( PBT) as the starting polyether,branching unit of trifunctional as intiator,PBT with a branched structure ( B-PBT) was synthesized by nucleophilic addition reaction under effect of a certain cata-lyst.The structure,viscosity properties,thermal stability and mechanical properties of the target product were characterized by FTIR, 1H-NMR,viscosity measurements,DSC,TG and tensile test. The results showed that the target product was a kind of azide ether with branched structure.The viscosity of B-PBT (15000 mPa·s/50℃) was significantly lower than that of PBT (23828 mPa· s/50 ℃) . The B-PBT has great thermal stability after branching units were introduced, where the decomposition heat release reached 1481 J/g. The thermal decomposition of B-PBT could be divided into two stages,namely thermal decomposition of the azi-do,scission of branching units and backbone into small molecules.Moreover,the B-PBT elastomers exhibits better mechanical prop-erties (σb=5.29 MPa,εb=516.42%) .
Keywords:3  3-bis( azidomethyl) oxetane/tetrahydrofuran  branched  viscosity  thermal stability
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