三氨基胍叠氮酸盐的非水相合成研究

Synthesis of Triaminoguanidinum Azide in Non-aquious Medium

在非水介质中用游离三氨基胍 (TAG)与通过离子交换树脂新生成的HN3进行中和反应 ,制备了三氨基胍叠氮酸盐 (TAZ)。实验证明 ,在甲醇中磺酸树脂与NaN3可定量生成HN3,且易分离 ,可避免将无机盐带入TAZ产品中。

Triaminoguanidinum azide (TAZ)is a promising ingredient for developing propellants with high specific impulse,low combustion temperature and low smoke used in missile or electrothermal chemical guns. The authors synthesized triaminoguanidinum nitrate (TAGN) and then transformed it into TAZ by reaction of sodium azide (NaN 3) with a kation exchange resin,but it was inevitable to leave some solid impurities like unreacted NaN 3 and the by product,NaNO 3,in the final product,and the yield of TAZ is only 23% based on TAGN. Therefore,this method is not beneficial to industrial production. In order to avoid the trouble above,the authors synthesized TAZ in non aqueous medium by the reaction of free triaminoguanidinum (TAG) with the fresh acid of HN 3 formed by ion exchange resin and NaN 3. The experimental results indicate that the reaction of sulfonate resin and NaN 3 in methanol can quantitatively produce HN 3 which is easy to be separated out and then react with pure TAG. This way,therefore,is promising to be used as an industrial procedure avoiding inorganic salts remained in the final TAZ product. The neutralization of TAG and HN 3 should be theoretically complete,but the yield of TAZ is only increase to 73.5% and 50% based on TAG and TAGN,respectively. The reason of incomplete neutralization should be further researched.