3,5⁃二甲基⁃4⁃羟苯基五唑中试合成工艺

Pilot Synthesis Techniques of 3,5⁃Dimethyl⁃4⁃hydroxyphenylpentazole

为了实现五唑前驱体3,5‑二甲基‑4‑羟苯基五唑(HPP)的规模化生产,最终实现五唑阴离子基含能材料的工程化应用,在现有实验室级别合成方法的基础上,利用10 L和100 L中试合成设备,对HPP的中试放大合成工艺进行了研究。分别研究了3,5‑二甲基‑4‑羟基苯胺盐酸盐(DAC)纯度、亚硝酸钠和叠氮化钠水溶液滴加速度以及投料量对HPP产量或产出比的影响。结果表明,在一定范围内,亚硝酸钠水溶液和叠氮化钠水溶液滴加总时间增加,HPP的产量也随之增加,到达一定值后,继续增加滴加时间并不会增加HPP产量;DAC的纯度对HPP的产量有较大影响,纯度越高,副反应越少,产量越高;另外,随着合成规模扩大,HPP产量增加,但是产出比却下降。投料量达到6 kg时,批量产出可达11.5 kg,但产出比低至1.91。

For achieving engineering application of pentazolium anionic energetic materials,it is necessary to realize large‑scale production of 3,5‑dimethyl‑4‑hydroxyphenylpentazole(HPP)as the precursor of pentazole.The pilot synthesis techniques of HPP were performed based on accessibly lab‑leveled method using 10 L and 100 L reactors for scale‑up experiments.The drop‑ping time of aqueous solutions of sodium nitrite and sodium azide,the purity and the feeding mass of 3,5‑dimethyl‑4‑hydroxyan‑iline hydrochloride(DAC),on the production of HPP were investigated.Results indicate that HPP production increases with the increasing of the total dropping time of sodium nitrite aqueous solution and sodium azide aqueous solution.After a certain val‑ue,the production of HPP remains.The purity of DAC affects the HPP production significantly that the production increases with the increasing of purity.With the scale up,HPP production increases along with the reducing of production ratio.With the feed‑ing mass of DAC reached to 6 kg,a batch of product increased to 11.5 kg as well as the production rate decreased to 1.91.