硝酸法控制结晶制备硝基胍  

Preparation of Nitroguanidine with Nitrate Method Based on Controlled Crystallization

作　　者：罗志龙[1] 康超[1] 徐其鹏[1] 邹高兴[1] 陈超[1] 杨毅[1] 

机构地区：[1]西安近代化学研究所,陕西西安710065

出　　处：《精细化工》2016年第9期1010-1013,共4页Fine Chemicals

基　　金：兵器装备预先研究基金(40406040203);基础产品创新火炸药专项~~

摘　　要：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 production process, a new process was used to synthesize nitroguanidine （NQ） using a nitrate method. The product was directly obtained by controlled crystallization from the crystallization reaction liquid, and its average grain size, acidity and purity could all meet the military requirements. When the stirring rate was 350 r/min, crystallization temperature was 271 K,dropping speed of dilution solution was 2 mL/min and crystal growing time was 90 minutes,the resulting NQ had an average grain size between 3 μm to 6 μm, its acidity was less than 0. 05 % and purity（HPLC） was more than 99.2%. The crystal morphology of the product prepared by controlled crystallization was compared with the crude NQ by SEM ,the result shows that controlled crystallization product present granular without refining, moreover, it has better compactness and homogeneity.

关 键 词：硝基胍 控制结晶 工艺条件 晶体形貌 分离技术 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术]