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为简化生产工艺,在硝酸法制备硝基胍(NQ)过程中,采用控制结晶技术直接从结晶反应液中制得了平均粒度、酸度和纯度均满足军用要求的硝基胍产品。结果表明:在搅拌速率350 r/min、结晶温度271 K、溶析液滴加速率2.0 m L/min、养晶时间90 min的工艺条件下制得的产品指标最优,产品粒度范围为3~6μm,酸度≤0.05%,纯度(HPLC)≥99.2%;经扫描电镜分析对比了该工艺所得产品与粗品硝基胍重结晶工艺的产品晶体形貌,结果显示:硝酸法控制结晶制备硝基胍未经精制即呈短棒颗粒状,且具有更好的致密性和均匀性。
In order to simplify the process of production of nitroguanidine (NQ), nitroguanidine products with average particle size, acidity and purity meeting the military requirements were prepared directly from the crystallization reaction liquid by controlled crystallization technology. The results showed that the optimal product index was obtained under the conditions of 350 r / min stirring speed, 271 K crystallization temperature, 2.0 mL / min stirring speed and 90 min holding time, and the product range was 3 ~ 6μm, acidity≤0.05%, purity (HPLC) ≥99.2%. The crystal morphology of the products obtained by this process and the crude nitroguanidine recrystallization process were analyzed by scanning electron microscopy. The results showed that nitric acid Guanidine was short rod granulation without refining, and has better compactness and uniformity.