N-丁基硝氧乙基硝胺所含杂质分析及其稳定性研究

Analysis of impurities in Bu-NENA and its influence on stability

采用液-质联用仪(LC-MS)、高效液相色谱(HPLC),对不同批次N-丁基硝氧乙基硝胺(Bu-NENA)进行了组分分析。通过加速老化试验,研究了Bu-NENA酸值及纯度的变化规律,综合分析了Bu-NENA内杂质产生的机理。同时,开展了不同中定剂对Bu-NENA使用过程中的稳定性影响研究。分析结果表明,Bu-NENA中主要杂质成分为丁基羟乙基硝胺和丁基乙酸乙基硝胺;丁基乙酸乙基硝胺为Bu-NENA合成时会产生的副产物;Bu-NENA遇水发生水解反应,产生杂质丁基羟乙基硝胺,同时其酸值增加,纯度下降,影响其使用性能。为了确保Bu-NENA使用性能,需要控制合成过程,减少副产物的产生;同时,严格控制使用、贮存等环境中的水分。因此,同时使用中定剂MENA、MNA,可以有效抑制Bu-NENA的老化分解。文中筛选出了合适的中定剂,为Bu-NENA的使用提供了理论支撑,以更好地进行优化设计,对实际生产具有重要的意义。

The components of Bu-NENA from different batches were analyzed by LC-MS and HPLC.Through accelerated aging test,the change rules of acid value and purity of Bu-NENA was studied,and the formation mechanism of impurities in Bu-NENA was analyzed.The effect of different centralites on the stability of Bu-NENA was studied.The results show that the main impurities in Bu-NENA are butyl hydroxyethyl nitramine and ethyl butylacetate nitramine.Butylacethyl nitramine is a byproduct of Bu-NENA synthesis.The ethyl butylacetate nitramine can be produced during the hydrolysis reaction of Bu-NENA.Its acid will increase and its purity will decrease at the same time.These changes will affect the service performance of Bu-NENA.Therefore,in order to ensure the service performance of Bu-NENA,it is necessary to control the synthesis process of Bu-NENA to reduce the production of byproducts,and strictly control the moisture in the use and storage environment.At the same time,the use of centralite MENA and MNA can obviously inhibit the aging decomposition of Bu-NENA.In this paper,a suitable centralite is selected,which provides a theoretical support for the use of Bu-NENA,so as to better optimize the design,which is of great significance to the actual production.